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# Test Plan for Environmental Protection Agency (EPA) Information Collection Request (ICR)

Prepared for:

Shintech Louisiana LLC

Test Scheduled for: August, 2014

Test Location:

Plaquemine Plant Plaquemine, Louisiana LDEQ Permit No. 1280-00118-V4

Prepared by:

Weston Solutions, Inc. Integrated Air Services 5599 San Felipe, Suite 700 Houston, TX 77056

24 July 2014

Valid through November 2014

This test plan has been prepared by Weston So lutions, Inc. (WESTON) for the exclusive use of Shintech Louisiana LLC (Shintech) and affilia ted companies, and WESTON. WESTON recognizes that a copy of this protocol may b ecome public record under EPA authority.

This document may be shared with regulatory agen cies having jurisdiction ove r the tested source. Otherwise, this document may not be released to, or used by others, without the advance written approval of WESTON.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Section Page No.

1. INTRODUCTION.................................................................................................... 5

2. OBJECTIVE AND SUMMARY OF THE EMISSION TEST PROGRAM ...... 5

3. SOURCE DESCRIPTION AND OP ERATING CONDITIONS ........................ 7 Facility Overview

.................................................................................................................... 7 3.1.

PVC Unit and Supporting Facilities

........................................................................................ 8 3.2.

VCM Unit

............................................................................................................................... . 9 3.3.

Control Devices

.................................................................................................................... 10 3.4.



### 4. TEST MATRIX & SAMPLING LOCATIONS .................................................. 11

5. TEST METHODS .................................................................................................. 13

6. PROCESS DATA REQUIREMENTS ................................................................. 19

7. QUALITY CONTROL PROCEDURES AND AUDITS ................................... 19

8. REPORTING FORMAT AND REPORTING UNITS ...................................... 20

9. PLANT DIRECTIONS, ENTRY, & SAFETY REQUIREMENTS .................. 23

10. TEST PROGRAM PERSONNEL & RESPONSIBILITIES ............................. 24

11. TEST PROGRAM SCHEDULE .......................................................................... 26

12. SOURCE TESTING METHODOLOGY ............................................................ 26
Volumetric Flow Rate

........................................................................................................... 26 12.1.

12.2 Oxygen/Carbon Dioxide (Instrumental)

............................................................................... 27

12.3 Hydrogen Chloride (Table 1.1 Compound List)

.................................................................... 28

12.4 Formaldehyde, Methanol and Ethylene Glycol (Table 1.5 Compound List)

........................ 30

12.5 Semivolat ile Organic Compounds (Table 1.4 Compound List, Site Specific HAP)

............... 34

12.6 Total Hydrocarbon Concentrations (Table 1.1 Compound List, 30

‐ Day Monitoring)

......... 39

12.7 Volatile Organic Comp ounds (SW846 Method 0031) (Table 1.3 Compound List)

............... 42

12.8 Speciated HAP

– Direct Interface (Table 1.1 Compound List, Site Specific HAP)................. 46



### 13. LABORATORY SAMPLE SUMMARY ............................................................. 50

14. VOST DETECTION LIMITS .............................................................................. 52

APPENDIX A - EPA ICR LE TTER – MAY 15, 2014 .................................................................. 56Test Plan for EPA ICR – Shintech Louisiana LLC

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### APPENDIX B - JULY 14, 2014 EPA EMAI L REGARDING PCB TESTING ..................... 60

APPENDIX C - ENCLOSURE 1, ATTACHMENT B AND C .................................................... 66

List of Tables and Figures

Table 2-1 Initial ICR Test Program ..................................................................................... 6 Table 2-2 Thirty Day THC Monitoring Program ............................................................... 7 Table 4-1 Test Matrix & Sampling Locations, Shintech SCR Inlet ................................ 11 Table 4-2 Test Matrix & Sampling Loca tions, Shintech GTO Scrubber Stack ............ 12 Table 5-1 Enclosure 1 Attachment B Table Summary - Methodology ........................... 13 Table 5-2 Initial ICR Test Program – GTO Scrubber Stack Location .......................... 14 Table 5-3 Total Hydrocarbon 30-Day Test Program – GTO Scrubber Stack ............... 16 Table 5-4 Total Hydrocarbon 30-Day Test Program – SCR Control Device Inlet ........ 17
Table 5-5 Detection Limits .................................................................................................. 18 Table 8-1 Anticipated Organization for Shintech ICR Report ....................................... 21 Table 8-2 Anticipated Organization for Shi ntech ICR 30-Day THC Monitoring Rep . 22 Table 10-1 Test Program Personnel & Responsibilities ................................................... 24
Table 10-2 Shintech Contacts ............................................................................................. 24 Table 10-3 Analytical Support Contacts ............................................................................ 25
Table 11-1 Planned Test Schedule ...................................................................................... 26 Figure 12-3-1 EPA Method 26A Sampling Train ............................................................. 29 Figure 12-4-1 EPA Method 316 Sampling Train .............................................................. 32 Figure 12-5-1 EPA Method 0010 Sampling Train ............................................................ 35 Figure 12-5-2 Sample Recovery Proce dures for Method 0010 Sampling Trains .......... 36 Table 12-5-1 Method 0010 Reagent Blank Samples ......................................................... 37 Table 12-5-2 Organic Glassware Cleaning Procedure ..................................................... 38 Figure 12-6-1 EPA M25A Samling Configuration ............................................................ 41 Figure 12-7-1 EPA Method 0031 Volatile Organic Sampling Train (VOST) ................ 43 Figure 12-8-1 EPA Method 18 Sampling Configuration .................................................. 48 Table 13-1 Sample Collection Summary ...................................................................... 50Test Plan for EPA ICR – Shintech Louisiana LLC

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### List of Acronyms

C 2 

### H 6 

### .............................................................................................................................. ... Ethane
CH 4 

### .............................................................................................................................. . Methane DSCM ............................................................................................ Dry Standard Cubic Meter EDC ........................................................................................................... Ethylene Dichlo ride EPA .................................................................................... Environmental Protection Agency
FID .................................................................................................. Flame Ionization Detect or GC ......................................................................................................... Gas Chromatograph y GPC .................................................................................... Gel Permeation Chromatography
GTO ....................................................................................................... Gas Thermal Oxidize r HAPs ................................................................................................. Hazardous Air Pollutants HCl ............................................................................................................. Hydrogen Chl oride ICR ........................................................................................ Information Collection Request
MDL ............................................................................................... Minumum Detection Limit
MACT .................................................................. Maximum Achievab le Control Technology
NMNE ........................................................................................... Non-Methane / Non-Ethane
O 2 

### ............................................................................................................................. .... Oxygen PCBs ................................................................................................ Polychorinated Byphenyls RDL ................................................................................................ Reporting Detection Limit SCR ............................................................................................ Selective Catalytic Reduction
TBD ............................................................................................................... To Be Deter mined THC ........................................................................................................... Total Hydrocarb ons VOC ........................................................................................... Volatile Organic CompoundsTest Plan for EPA ICR – Shintech Louisiana LLC

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### 1. Introduction

Weston Solutions, Inc. (WESTON ® ) has been retained by Shintech Louisiana LLC (Shintech) to conduct emission testing at its Plaquemine facility in Plaquemine , Louisiana. This test program has been initiated in response to a letter dated May 15, 2014 from the EPA in regards to an ICR for PVC manufacturing facilities.

This test plan has been prepared at the request Shintech and has been forma tted to clearly and efficiently satisfy the requirements set forth in Section 12.3 of ASTM D7036-04, Standard Practice for Competence of Air Emission Testing Bodies . WESTON certifies that at the date of this transmittal it operates in conformance with ASTM D7036-04 standard and is accredited by th e Louisiana Environmental Laboratory Accreditation Program (LELAP) effective December 2001 and valid through 30 June 2015.

The technical approach described in this test plan is valid for 120 days from the revision date. Note that regulations and test methods are always evolving. Shou ld regulations or test methods affecting this test program change within the period of test plan validity, WESTON will advise Shintech.

The project schedule described in this test plan is valid through November 2014. WESTON will confirm or update the project schedule via email. A formally revi sed and reissued test plan will not be provided unless specifically requested and authorized.

The compounds of interest for the ICR are outlined in the May 15, 2014 letter received by Shintech from the EPA. The letter includes six enclosures, with “Enc losure 1” consisting of the document “Maximum Achievable Control Technology (MACT) Standards Development Information Collection Request” with tables 1.1 through 1.6 outlining compounds of interest as well as describing test methodologies and reporting requirements. WESTON will use the services of two anal ytical laboratories to collect and/or analyze the samples as outlined in the ICR request.

WESTON’s contract laboratory will be Enthalpy Analyti cal, Inc. (Enthalpy) for the compounds of interest identified in Table 1.1, 1.4, 1.5, and site specifi c HAP compounds, as identified and labeled in the PVC ICR collection request and subsequent Ma y 14, 2014 letter from the EPA to Shin tech. Enthalpy is accredited by
the NELAC institute.

WESTON’s contract laboratory will be Maxxam Analyti cs Inc. (Maxxam) for the compounds of interest identified in Table 1.3 of the ICR request. Maxxam is accredited by the NELAC institute.

Shintech considered the addition of PCBs to the list of site specific HAP as it was previous detected under a previous 114D request. Shintech, via the Vinyl Institute , made an inquiry to US EPA (Jodi Howard)if testing of this compound was necessary. US EPA responded that testing for PCB was not necessary and, as a result, is not included as parameter as part of this test plan . See Appendix B for the e-mail correspondence regarding
this issue.



### 2. Objective and Summary of th e Emission Test Program

The ICR request for PVC manufacturing facilities consists of two distinct testing programs. One program consists of performing three test runs for various com pounds as outlined in Tables 1.1-1.5 of the ICR request. The second program is outlined in Table 1.6 of the doc ument, and consists of performing thirty-days of continual monitoring for oxygen, moisture, total hydro carbons and methane. Ethane measurements will also beTest Plan for EPA ICR – Shintech Louisiana LLC

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Initial ICR Compliance Test Program

The emission testing program will be conducted to comply with the EPA ICR request as outlined in the May 15, 2014 letter sent to Shintech from the EPA. The test program will involve the measurement of volumetric flow, gas composition, and select HAPs using EPA Met hods 1, 2, 3A, 4, 25A, 26A, 316 (modified), SW-846 Methods 0010, and 0031. Three test runs will be performed for all parameters.



### Table 2-1 Initial ICR Test Program

Reference Method/Parameter Process Location

GTO Scrubber Stack

Flowrate X

Moisture X
Gas Composition (M3A) X
Hydrogen Chloride X
Total Hydrocarbons X

Methane X

Ethane X
Speciated HAP X

Total Hydrocarbon 30-Day Monitoring Test Program

As per the instructions found in the EPA letter, the “T otal Hydrocarbon 30-Day Monitoring Test Program”, as described in the next paragraph, will be initiated before the start of the initial ICR compliance test program and data will be collected concurrently with the main IC R test program. Table 2-1 summarizes the initial ICR test
parameters.

Total hydrocarbons (THC), methane (CH 4 ), oxygen (O 2 ), and moisture will be monitored and recorded for thirty consecutive days as outlined in Table 1.6 of the ICR Enclosure 1, A ttachment B. Although not required by the ICR, ethane (C 2 H 6 ) will also be recorded. Due to the uni que configuration of the process at the Plaquemine facility, the monitoring will be performed at two locations. The scrubber stack will be monitored at the outlet to the stack. Additionally, the inlet to th e SCR will be monitored to provide a baseline reading of THC, methane and ethane before the selective cataly tic reduction (SCR) process. Due to the temperature requirements of the SCR, the gas stream entering the de vice must be heated by natural gas burners. It is anticipated that the THC levels at the stack location ma y be biased high due to this heating process. Table 2-2 summarizes the thirty day THC monitoring program test parameters.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Table 2-2 Thirty Day THC Monitoring Program

Reference Method/Parameter Process Location

Inlet to SCR GTO Scrubber Stack
Total Hydrocarbons X X

Methane X X

Ethane (1) X X
Oxygen X X
Moisture (Method 4, Once per Day) X
Moisture (Saturation Temperature, Once per Day) X

1 Ethane measurements are for engineering purpo ses and are not a requirement of the ICR program



### 3. Source Description and Operating Conditions

Facility Overview 3.1. Shintech Louisiana, LLC (Shintech), a wholly owned subsidiary of C-K Tech, Inc., is currently operating the Shintech Plaquemine Plant 1 (SPP-1) on the west bank of the Mississippi River near Plaquemine, Louisiana in Iberville Parish. SPP-1 is part of the Shintech Plaquemine Plant Complex, which includes the following
facilities:

 SPP-1 – Authorized by Prevention of Significant Deterioration (PSD) Permit No. PSD-LA-709(M-1) and Clean Air Act (CAA) Title V Permit No. 1280-00118-V4 issued on May 9, 2012 by the Louisiana Department of Environmental Quality (LDEQ)

 Hydrochloric Acid Plant (HAPF-1) – Authori zed by PSD Permit No. PSD-LA-738 and CAA Title V Permit No. 3064-V1 issued on June 29, 2012 by the LDEQ

 SPP-2 – Authorized by PSD Permit No. PSD-LA-731 and CAA Title V Permit No. 3063-V2 issued on July 31, 2012 by the LDEQ

 HAPF-2 – Authorized by PSD Permit No. PSD-LA- 739 and CAA Title V Permit No. 3066-V1 issued on June 29, 2012 by the LDEQTest Plan for EPA ICR – Shintech Louisiana LLC

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### PVC Unit and Supporting Facilities 3.2.Test Plan for EPA ICR – Shintech Louisiana LLC

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### VCM Unit 3.3.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Control Devices 3.4. Thermal destruction is accomplished in Gas Thermal Oxidi zers (GTOs). Fresh air is forced into the GTO by a blower, where it supports combustion of natural gas to produce heat. An operating temperature of 980°C is
maintained in the Thermal Oxidizer combustion chamber, which provides thorough decomposition of residual EDC, VCM, and other organic chemicals in the vent st reams. The products of this decomposition are CO2, HCL, and small amounts of CL2 and NOx. Steam is injected into the combustion chamber to encourage the
conversion of elemental chlorine to HCL.

Vapors in the combustion chamber pass through the tube side of MHE551A/B boiler for heat recovery before entering the Vent Scrubbing Subsystem. The recovered heat produces steam for use in the plant as a utility.

These vents enter the Scrubber below its packed section and flow upwards through a circulating stream of
caustic water. The caustic reacts with HCL to make salt and with the chlorine to make bleach. A small flow
of sodium thiosulfate is added to the caustic water and converts the bleach to harmless sodium sulfate. A constant makeup of caustic is added to replace what is lost to neutralization. A steady liquid purge to the Copper Removal unit removes accumulated salt, and deminera lized water is added to replace the level lost to the purge and evaporation.

Vents leaving the Scrubber, now essentially free of HCL a nd chlorine, enter the NOx Decomposer area. First they pass through the GTO Demister for droplet removal, th en exit to the inlet side of the Vent Gas heater for warming, where a natural gas flame heats them to operating temperature. On their way to the NOx Decomposer Reactor (SCR), atomized ammonia water is sprayed into the vent stream and mixed by static mixers. Within the NOx Decomposer, any nitrogen oxides react on th e surface of the SCR catalyst with ammonia to produce water and nitrogen. Hot vents exiting the SCR enter the Vent Gas Reheater where heat is recovered back to the SCR feed prior to these vents being released to the atmosphere.

The purpose of the NOx Decomposer subsystem is to rem ove NOx in flue gases to comply with environmental regulations.Test Plan for EPA ICR – Shintech Louisiana LLC

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### 4. Test Matrix & Sampling Locations

Table 4-1 summarizes information about the sampling locations and source gas characteristics (matrix) at the
test location.



### Table 4-1 Test Matrix & Sampling Loca tions, Shintech SCR Control Device Inlet

Characteristic Available Information

Duct Geometry Circular

Duct Size, inches ~40
Port Size, inches >10 (Valve Assembly)

No. of Ports & Placement 1, Vertical Plane
Distance to Upstream Disturbance, feet TBD
Distance to Downstream Disturbance, feet TBD
Flow, ACFM < 14,149
Flow, DSCFM < 8,490 (based on scrubber)
Temperature, °F ~135
Moisture, % 17
Entrained Droplets? Possible (Saturated)

O 2 , % ~8

CO 2 , % ~8

N2, % >80 (assumed)

The test program involves the measurements of THC, et hane and methane from a location that has not been previously tested. An assumption has been made that concentrations of THC and methane will be lower at
the SCR inlet location than at the stack. Previous t esting at the stack indicates concentrations of THC have averaged as much as 16 ppmv @ 3% O 2 , concentrations of methane have averaged as high as 31 ppmvw @
3% O 2 , oxygen has averaged approximately 8% (dry), and carbon dioxide has averaged approximately 7% (dry). Once on site, WESTON will verify source dimensions. Volumetric flow rates will NOT be
determined at the SCR inlet location. Shintech personnel have indicated that the source location is saturated. Temperature measurements will be recorded and used to calculate the percent moisture of the
location based on saturation.

TBD=To Be DeterminedTest Plan for EPA ICR – Shintech Louisiana LLC

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### Table 4-2 Test Matrix & Sampling Lo cations, Shintech GTO Scrubber Stack

Characteristic Available Information

Duct Geometry Circular

Duct Size, inches 71.625
Port Size, inches 4”, 13.25” deep

No. of Ports & Placement 2, Ver tical Plane, 90 degrees apart
Distance to Upstream Disturbance, feet 18
Distance to Downstream Disturbance, feet 45

Flow, ACFM 14,149

Flow, DSCFM 8,490
Temperature, °F 328
Moisture, % 11.3
Entrained Droplets? No

O 2 , % 8.0

CO 2 , % 6.8
N2, % >80 (assumed)

Previous data is available for the GTO (Stack) outlet. Previous data indicates that the location is not stratified, cyclonic, or saturated. WESTON will verify source dimensions, stratification, and the absence of cyclonic flow.Test Plan for EPA ICR – Shintech Louisiana LLC

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### 5. Test Methods

This test program involves simultaneous testing using is okinetic methods for several of the test parameters. Each isokinetic method will generate its own set of volumetric flow data which will be used for emission calculations. Because simultaneous testing will involve the use of multiple ports, volumetric flow data for simultaneous methods may differ slightly.

Tables 5-1 through 5-4 provide information about the test methods that will be used for the test program.



### Table 5-1 Enclosure 1 Attachment B Table Summary – Methodology

Enclosure 1
Attachment B Table Pollutant Collection Method Contracted Laboratory

Table 1.1 Hydrogen Chloride (HCl) US EPA M26A Enthalpy

THC US EPA M25A ‐ Methane US EPA M18 Direct Interface Enthalpy Vinyl Chloride ‐ Not Requested NA Dioxins/Furans ‐ Not Requested NA
Table 1.2 Dioxin/Furan Congener List ‐ Not Applicable NA
Table 1.3 Table 1.3 Speciated HAP List SW

‐ 846 M0031 Maxxam
Table 1.4 Table 1.4 Speciated HAP List SW

‐ 846 M0010 Enthalpy

Table 1.5 Ethylene glycol, Formaldehyde, Methanol US EPA M316
US EPA M316 Modified Enthalpy

Acetaldehyde, 1,3

‐ Butadiene, Chlorobenzene, Chloromethane, Cumene, Ethylbenzene, 1,1,2,2,

‐ Tetrachloroethane, 2,2,4

‐ Trimethylpentane, Vinyl
acetate, Vinyl bromide, Xylenes (

‐ m/p, ‐ o) US EPA M18 Direct Interface Enthalpy

Site Specific Hap Carbon tetrachloride, Tetrachloroethylene, Trichloroethylene, Methyl isobutyl ketone US EPA M18 Direct Interface Enthalpy

Dichloroethyl ether, 1,4

‐ Dichlorobenzene SW

‐ 846 M0010 EnthalpyTest Plan for EPA ICR – Shintech Louisiana LLC

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### Table 5-2 Initial ICR Test Program – GTO Scrubber Stack Location
Method No. Parameter Condition 1, Full Load

1 Traverse Points -- Test Method EPA Reference Method 1
Number of Runs Stack measured at outset, traverse points selected Run Duration, Minutes NA Simultaneous with Methods 2, 3A, 4, 26A, 316(Modified), 0010 Reporting Units Each

2 Volumetric Flow -- Test Method EPA Reference Method 2 Number of Runs 3 per test Run Duration, Minutes Corresponds to the length of simultaneous test Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 Reporting Units ACFM/DSCFM

3A Gas Composition (O 2 , CO 2 , N 2 ) -- Test Method EPA Reference Method 3A Number of Runs 3 per test Run Duration, Minutes Corresponds to the length of simultaneous test Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 Reporting Units %

4 Moisture -- Test Method EPA Reference Method 4 Number of Runs 3 per test Run Duration, Minutes Corresponds to the length of simultaneous test Simultaneous with Methods 1, 3A, 4, 18, 25A, 26A, 316 (Modified), 0010, 0031 Reporting Units %

18 Methane, Site Specific HAPS by GC -- Test Method EPA Reference Method 18 Number of Runs 3 per test Run Duration, Minutes 240 Simultaneous with Methods 1, 2, 3A, 4, 25A, 0010, 316 (Modified), 0031 Reporting Units ppmvd@3% O 2

25A *1 Total Hydrocarbons (THC) -- Test Method EPA Reference Method 25A
Number of Runs 3 per test Run Duration, Minutes 240
Simultaneous with Methods 1, 2, 3A, 4, 18, 0010 Reporting Units ppmvd @ 3% O 2 (as propane)

26A Hydrogen Chloride (HCl) -- Test Method EPA Reference Method 26A Number of Runs 3 per test Run Duration, Minutes 120 (2 dscm) Simultaneous with Methods 1, 2, 3A, 4, 18, 25A, 316 (Modified), 0031 Reporting Units ppmvd@3% O 2

316 Formaldehyde, Methanol, Ethylene Glycol --

Test Method EPA Reference Method 316 Modified
Number of Runs 3 Run Duration, Minutes 60 Simultaneous with Methods 1, 2, 3A, 4, 18, 25A, 316,26A, 0031 Reporting Units ppmvd@3% O 2 Reporting Units ppmvd @ 3% O 2Test Plan for EPA ICR – Shintech Louisiana LLC

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‐ 2 Initial ICR Test Program

– GTO Scrubber Stack Location Cont’d

0010 Semivolatile Organic Compounds (SVOCs) --

Test Method SW 846 Method 0010, Prep SW 846 3542, Analysis 8270D
Number of Runs 3 per test Run Duration, Minutes 180 (3 dscm)
Simultaneous with Parameter No. 1, 2, 3A, 4, 18, 25A Reporting Units ppmvd @ 3% O 2

0031 Volatile Organic HAPs -- Test Method SW 846 Method 0031, Preparation SW 846 Method 5041A, Analysis SW 846 M8260B Number of Runs 3 per test Run Duration, Minutes 80 (1L/min) Simultaneous with Parameter No. 1, 2, 3, 4, 18, 23, 25A, 26A, 316 (Modified) Reporting Units ppmvd @ 3% O 2 *1 The 30

‐ day monitoring program for total hydrocarbons will be initiated before the start of the general ICR

data collection as outlined in the table above. Calibrations will be performed before and after the four

hour test runs to bracket the THC data that will be utilized to satisfy Table 1.1 of the ICR request. The

relevant time periods of the 30

‐ day monitoring data bracketed by calibrations will also be utilized for the

purposes of the four hour ICR test runs using the same THC data signal/analyzer.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Table 5-3 Total Hydrocarbon 30-Day Test Program – GTO Scrubber Stack Location

Method No. Parameter

3A Gas Composition (O 2 , CO 2 , N 2 ) -- Test Method EPA Reference Method 3A Number of Runs 30 Days Continuous (1) Run Duration, Minutes Calibrations at a minimum daily Simultaneous with Methods 3A, 4, 18, 25A
Simultaneous with Source ID SCR Inlet Reporting Units %

4 Moisture -- Test Method EPA Reference Method 4 Number of Runs 1 per Day Run Duration, Minutes 1 hr Simultaneous with Methods 3A, 18, 25A
Simultaneous with Source ID SCR Inlet Reporting Units %

18/25A (2) Methane/Ethane Test Method EPA Reference Method 25A using chromatographic column Number of Runs 30 Days Continuous (1) Run Duration, Minutes Calibrations at a minimum daily Simultaneous with Parameter No. 3A, 4, 18, 25A
Simultaneous with Source ID SCR Inlet Reporting Units ppmvd @ 3% O 2 (as methane)

25A THC

Test Method EPA Reference Method 25A

Number of Runs 30 Days Continuous (1)

Run Duration, Minutes Calibrations at a minimum daily

Simultaneous with Methods 3A, 18, 25A

Simultaneous with Source ID SCR Inlet Reporting Units ppmvd @ 3% O 2 (as propane)

1 Thirty days of data will be collected on the unit. If sampling time is interrupted due to weather, analyzer failure, or unforeseen events the program will be extended until the data objective has been met.

2 A VIG 210 hydrocarbon analyzer will be used to measure THC, methane, and ethane at the inlet to the SCR

control device and at the outlet stack location. This analyzer utilizes two FID detectors. One FID

detector measures total hydrocarbons. The second FID detector is attached to a chromatographic column

that separates methane and ethane from the other hydrocarbons and periodically reports their value.

The ICR Enclosure 1 document, Table 1.6, references an analyzer using these principles in the “Alternate

Method” column.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Table 5-4 Total Hydrocarbon 30-Day Test Pr ogram – SCR Control Device Inlet Location

Method No. Parameter

3A Gas Composition (O 2 , CO 2 , N 2 ) -- Test Method EPA Reference Method 3A Number of Runs 30 Days Continuous (1) Run Duration, Minutes Calibrations at a minimum daily Simultaneous with Methods 3A, 4, 18, 25A Simultaneous with Source ID GTO (Stack) Outlet Reporting Units %

4 Moisture -- Test Method EPA Reference Method 4 (psychrometric chart) Number of Runs Calculated from Temperature, Saturated Run Duration, Minutes NA Simultaneous with Methods 3A, 18, 25A Simultaneous with Source ID GTO (Stack) Outlet Reporting Units %

18/25A (2) Methane/Ethane Test Method EPA Reference Method 25A using chromatographic column Number of Runs 30 Days Continuous (1) Run Duration, Minutes Calibrations at a minimum daily Simultaneous with Parameter No. 3A, 4, 18, 25A
Simultaneous with Source ID SCR Inlet Reporting Units ppmvd @ 3% O 2 (as methane)

25A THC
Test Method EPA Reference Method 25A
Modifications None Number of Runs 30 Days Continuous (1) Run Duration, Minutes Calibrations at a minimum daily Simultaneous with Methods 3A, 18, 25A Simultaneous with Source ID GTO (Stack) Outlet Reporting Units ppmvd @ 3% O 2 (as propane)

1 Thirty days of data will be collected on the unit. If sampling time is interrupted due to weather, analyzer failure, or unforeseen events the program will be extended until the data objective has been met.

2 A VIG 210 hydrocarbon analyzer will be used to measure THC, methane, and ethane at the inlet to the SCR

control device and at the outlet stack location. This analyzer utilizes two FID detectors. One FID

detector measures total hydrocarbons. The second FID detector is attached to a chromatographic column

that separates methane and ethane from the other hydrocarbons and periodically reports their value.

The ICR Enclosure 1 document, Table 1.6, references an analyzer using these principles in the “Alternate

Method” column.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Reporting and Calculating Method Detection Limits

Tables 1.1-1.5 of the document “Enclosure 1 Attachment B” provide the units of measure for reporting. Section 2.0 of the ICR document titled “Enclosure 1 Attachment C” outlines the procedure for handling
detection limits for each test run and test series. S ection 3.0 of the same document outlines how data will be
submitted.

Detection limits for the various compounds are listed in Table 5-5. The detection limits are based on the theoretical sample volumes listed in Table 5-5. Actual detection limits may vary.



### Table 5-5 Detection Limits

Enclosure 1
Attachment B Table Pollutant Minimum Detection Limit (MDL) Minimum Sample
Volume

Table 1.1 Hydrogen Chloride (HCl) <15 ppb ( EPA M26A) 2 DSCM

THC US EPA M25A ‐ Methane .20

– 0.50 ppm (EPA M18) NA Vinyl Chloride ‐ Not Requested NA Dioxins/Furans ‐ Not Requested NA
Table 1.2 Dioxin/Furan Congener List ‐ Not Applicable NA
Table 1.3 Table 1.3 Speciated HAP List See Section 14 of Protocol 20L/Tube Set
Table 1.4 Table 1.4 Speciated HAP List <0.05 ppb (SW

‐ 846 M0010) 3 DSCM

Table 1.5 Ethylene glycol, Formaldehyde, Methanol 0.50  g/mL (EPA M316/EPA

M316 Modified 2 DSCM

Acetaldehyde, 1,3

‐ Butadiene, Chlorobenzene, Chloromethane, Cumene, Ethylbenzene, 1,1,2,2,

‐ Tetrachloroethane, 2,2,4

‐ Trimethylpentane, Vinyl
acetate, Vinyl bromide, Xylenes (

‐ m/p, ‐ o) .20

– 0.50 ppm (EPA M18) NA

Site Specific Hap Carbon tetrachloride, Tetrachloroethylene, Trichloroethylene, Methyl isobutyl ketone 0.20

– 0.50 ppm (EPA M18) NA

Dichloroethyl ether, 1,4

‐ Dichlorobenzene <0.05 ppb (SW

‐ 846 M0010) 3 DSCMTest Plan for EPA ICR – Shintech Louisiana LLC

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### 6. Process Data Requirements

Shintech will collect sufficient pro cess and fuel data to confirm operating conditions for each test. The
WESTON Test Team Leader will coordinate with a desi gnated Shintech representative before starting each run and upon completion of each run to (1) ensure that t esting is conducted under desi red conditions and (2) allow Shintech to flag process data appropriately. WESTON w ill include supplied Process Data in the Test Report. Per Enclosure 1, Attachment B of the ICR lette r, the following process data should be reported:

Type of resin being processed and the resin grade

Emissions control device(s) in use during the test

Control device operating or monito ring parameters (including, as appr opriate to the control device, flue gas flow rate, pressure drop, scrubber liquor pH, scrubber liquor flow rate, sorbent type and sorbent injection rate

Process parameters (such as percent oxygen)

The testing should be conducted while the PVC production process and any other non-PVC production process(es) that send emission streams to the same control device, is/are operating as close as possible to maximum mass loading of all HAP compounds to the c ontrol device and under “Normal” operation (page 2, paragraph 4, Enclosure 1, Attachment B)



### 7. Quality Control Procedures and Audits

Quality Control Procedures

The quality control procedures specified in the test methods described in Section 12.0 of this test plan apply to the test program.

The project reports will be reviewed by the WESTON technical director or designated WESTON quality assurance representative and the project manager prior to transmittal. Verification of these reviews will be indicated by signatures on the report tran smittal page and by initialing of the DPI control sheet. All data will be peer reviewed before submittal to any client representative.

Field data sheet entries and averages will be calculated and checked by a second person while onsite. Data sheets will be initialed and dated by the person performing the verification. Spreadsheet entries will be reviewed to include verification of laboratory data. Data package su bmittals will include the following: organized field data with descriptions of test problems and/or deviations, daily activity summaries describing delays encountered and names of regulatory observers and plant personnel present, copies of calibration records and spreadsheets as applicable.

The M0031 test train will be recovered in a separate mobile laboratory from the M0010 test train to avoid sample contamination from organic solvents used in the recovery of those sample trains.

Data from the 30-day total hydrocarbon monitoring program will be back ed up daily during the data collection period to WESTON data servers.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 20 of 66 WESTON may release measurement data while on site. Such data provided are considered “preliminary” and labeled accordingly. Final da ta are released following appropriate technical reviews.

Audit Materials

As this testing is not for compliance purposes, the audit sample for M26A (HCl) will not be requested, analyzed and is not required.



### 8. Reporting Format and Reporting Units

Overview

WESTON will prepare a comprehensive test report that follows the outline established in Section 15.3 of ASTM D 7036-04 and will satisfy requirements established by the EPA. Measurements will be reported in the units specified in Tables 5.1 – 5.3.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 21 of 66 Report Organization

The Emission Test Reports will be organized as follows:



### Table 8-1 Anticipated Organization for Shintech ICR Report

Section 1: Introduction (summary of test program objectives, personnel, and schedule)

Section 2: HAPs Results and Discussion (including summary of all test program results)

Section 3: Source Testing Methodology

Section 4: Process and Sampling Location Descriptions

Section 5: Quality Control Procedures

Appendix A: Detailed T est Data and Results

Appendix B: Field Data

Appendix C: Process Data

Appendix D: Laboratory Analytical Data

Appendix E: Quality Control Data

Appendix F: Example Calculations

Please note that the final outline may vary from this draft outline if there are changes in simultaneous testing requirements or test methods.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Table 8-2 Anticipated Organization fo r Shintech ICR 30-Day THC Monitoring

Table of Contents
Section 1: Introduction (summary of test program objectives, personnel, and schedule)

Section 2: Results and Discussion (including summary of all test program results)

Section 3: Source Testing Methodology

Section 4: Process and Sampling Location Description

Section 5: Quality Control Procedures

Appendix A: Detailed T est Data and Results

Appendix B: Field Data

Appendix C: Process Data

Appendix D: Quality Control Data

Appendix E: Example Calculations

Please note that the final outline may vary from this draft outline if there are changes in simultaneous testing requirements or test methods.Test Plan for EPA ICR – Shintech Louisiana LLC

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The initial ICR Scope test report will be submitted within six weeks after completion of the test program. A final report will be provided within one week of draft comments.

The 30-Day THC Monitoring test report will be submitted within four weeks after completion of the test program. A final report will be provided within one week of draft comments.

Report submittals will be in the form of hard copi es and electronic (PDF) copies. If requested, WESTON will assist Shintech in submitting the test data to EPA via the electronic reporting tool “ERT” as required in the ICR
documents.

Reports shall be sent to:

Mr. Thomas Andersen Shintech, Inc. 5618 East Hwy 332 Freeport, Texas 77541
tandersen@shin-tech.com



### 9. Plant Directions, Entry, & Safety Requirements

Driving Directions

The physical address for the Shintech Louisiana LLC Plaquemine Facility is:

Shintech Louisiana LLC

26270 Louisiana 405 Plaquemine, LA 70764

Entry

Check in at Security Gate 1.

The plant contact is Mr. Tim Gilder / Thomas Andersen.

Health & Safety

A site-specific health and safety (H&S) plan will be prepared for this project. All field team members are responsible for reading the health and safety plan and signing it prior to performing work in the field. The original, signed H&S plan must be retained in the office and a copy prepared for use in the field. The Field Team Leader is responsible for maintaining a copy of Material Safety Data Sheets at the project site and for enforcing compliance with the Health and Safety Plan. Any changes in field situations that may require amendment of the H&S plan while in the field must be documented and replaced in the original document.Test Plan for EPA ICR – Shintech Louisiana LLC

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### 10. Test Program Personnel & Responsibilities

Weston Organization

The WESTON project team for this effort consists of the following individuals with the indicated responsibilities:



### Table 10-1 Test Program Personnel & Responsibilities

Individual Cell Phone No . Responsibility Role

Wes Fritz 610-721-6419 Client Service Manager Project Direction
Jason Myers 512-658-4211 PM/SHSC/TTL Project Management
Paul Meeter 484-645-2626 TD/QA Quality/Technical Management

Donnie Fetzer 713-410-0966 TTM

Hunter Goodlett 334-750-1507 TTM

Jim Wallis 334-332-7127 TTM
Enthalpy Analyst ---- TTM Onsite GC Analysis

Ashley Bryant 334-338-5839 RC
Natalie Hornsby 334-466-5607 QA Responsibilities: PM = project manager, TD = technical di rector, TTL = test team leader, TTM = test team member, AS = analytical services, SH = Sample Handler, QA = qua lity assurance/quality control, RC = report coordinator, EC = equipment coordinator, SHSC = site health and safety coordinator

Client Organization

Key Client contacts are summarized below:



### Table 10-2 Shintech Contacts

Shintech Primary Shintech
Alternate

Name: Thomas Andersen Tim Gilder
Shipping Address 5618 Highway 332 East Freeport, TX 77541 26270 Louisiana 405 Plaquemine, LA 70764
Office Phone (979) 233-7861 ex t. 398 (225) 687-2105 ext. 5619
Mobile Phone (979) 236-5641 (225) 278-5593

E-mail: tandersen@shin-tech.com tgilder@shin-tech.comTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 25 of 66 Analytical Support Contacts

Analytical support for this project will be provided by the following laboratories:



### Table 10-3 Analytical Support Contacts
Lab: Enthalpy Analytical Maxxam Analytics

Contact: David Berkowitz Jim Jacklin/Clayton Johnson
Shipping Address: 800 Capitola Dr.
Durham, NC 27713 6740 Campobello Road Mississauga, ON Canada L5N2L8
Telephone: 919-850-4392 ext. 225 800-563-6266

Fax: 919-491-9841 905-817-5777

E-mail: David.Berkowitz@enthalpy.com jjacklin@maxxam.ca

Parameters: Table 1.1 (M26A, Methane), Table 1.4, Table 1.5, Site Specific HAPS Table 1.3 (M0031)

Turn-around Time 21-Day 21-DayTest Plan for EPA ICR – Shintech Louisiana LLC

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### 11. Test Program Schedule

Table 11-1 Planned Test Schedule

Day Date Activity

GTO Scrubber Stack SCR Inlet
1-2 10-11 Aug 2014 Travel to Site, begin setup

3 12 Aug 2014 Continue Set-up/Begin 30-Day THC Monitoring 30 Day THC Monitoring

4 13 Aug 2014 Test Run 1 / 30 Day THC Monitoring 30 Day THC Monitoring, Cont’d

5 14 Aug 2014 Test Run 2 / 30 Day THC Monitoring 30 Day THC Monitoring, Cont’d

6 15 Aug 2014 Test Run 3, Demobilize / 30 Day THC Monitoring 30 Day THC Monitoring, Cont’d

7-32 16 Aug – 10 Sept 2014 30 Day THC Monitori ng, Cont’d 30 Day THC Monitoring, Cont’d

30 8 Sept 2014 Laboratory Data Packages Due

‐ 33 11 Sept 2014 Demobilize 30 Day THC Monitoring 51 Sept 29, 2014 Main ICR Program Draft Report Due 61 Oct 8, 2014 30 Day THC Monitoring Program Draft Report Due - Nov 14, 2014 ICR Data Submission Deadline – EPA



### 12. Source Testing Methodology

The sampling methodologies to be used in the EPA ICR t est program are described in the following sections. Table 12-1 provides detailed informa tion regarding the sample fractions for each method and the reporting detection limits for the various analyses.



### Volumetric Flow Rate 12.1. Mass emission rates are calculated by multiplying measu red target analyte concentrations by calculated volumetric flow rates. Volumetric flow rates are calculated using measurement data obtained by EPA
Reference Methods 1-4.

The ductwork is measured at the sample location to the n earest 0.25 inch using a steel tape measure. Traverse points are selected in accordance with EPA Reference Method 1 on the basis of ductwork dimensions, geometry, and upstream and downstream disturbances. When a sample location does not meet EPA Reference Method 1 criteria, the maximum r ecommended number of traverse points is used.

Gas Velocity

The velocity of the gas stream is measured in acco rdance with EPA Reference Method 2 by reading the instantaneous velocity pressure with an inclined manometer at each traver se point using either a standard “P” type or an “S” type pitot tube. The stack pressure is calculated from th e measured static pressure of the stack and the ambient barometric pressure. The static pressure is measured by using the static side of the pitot tube, and the barometric pressure is measured usi ng a calibrated aneroid barometer. Magnahelic  gauges with
scales of 0 to 5 and 0 to 25 inches of water or an inclin ed manometer with a scale of 0 to 10 inches of water is used for velocity pressure measurements. Manometer sel ection is determined by the velocity pressure of theTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 27 of 66 gas stream. A manometer with a 0 to 0.25 inch scale may be used when the velocity pressure of the gas stream is less than 0.25 inches of water. By convention, any measured velocity pressures of less than 0.005 inches of water are recorded and reported as less than 0.005 inches of water. The stack temperature is measured with a calibrated thermocouple and pyrometer.

For low velocity pressure measurements (less than 0.005 inches of water) a digital manometer may be used to measure the velocity of the gas stream.

Gas Composition and Moisture Content

The moisture content of the gas stream is de termined using one of the following procedures:

 For sources requiring testing by EPA Reference or Test Methods 5, 8, 12, 13, 17, 23, 26A, 29, 0010, or 0011, moisture is determined by EPA Reference Method 4. At the conclusion of each run the volume of condensed moisture in the impingers of the sampling train is measured and used to calculate the moisture content of the gas stream.

 For sources with temperatures greater than 212 °F, the approximation tech nique described in EPA Reference Method 4 may be used with midget or full sized impingers to condense moisture before dry gas volume measurement.

 For sources with a temper ature of less than 212 °F, wet bulb/dr y bulb temperature measurements may be made, and the moisture content calculated using vapor pressure tables.

The molecular weight of the gas stream is calculated using the measured moisture, oxygen, and carbon dioxide concentrations. The balance of the gas stream is assu med to be nitrogen. The volumetric flow is then calculated at stack and standard conditions using the calculated molecular weight, the measured stack temperature, and measured velocity, stack and barometric pressures. Standard conditions are 68 °F and 29.92 inches of mercury and 0% moisture.

Data Acquisition and Reporting

Data are recorded at the time of collection on prepri nted data sheets. Calculations are performed (where possible) with verified preprogrammed calculators or spreadsheet software.

Quality Control

Quality control procedures for volumetric flow measuremen ts involve leak checks of pitot tubes, pitot tube
lines and manometers.

Data transfers are minimized. Data sheets are checked for completeness and accuracy. Calculations are verified by a second person.



### 12.2 Oxygen/Carbon Dioxide (Instrumental) Oxygen (O2) and carbon dioxide (CO2) testing is conducted in accordance with EPA Reference Method 3A. The sample is withdrawn continuously from the source through a heated probe, filter, and sample line to aTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 28 of 66 sample conditioner, which removes moisture from the g as stream. The sample is then transported to a paramagnetic O2/CO2 analyzer. The analyzer uses a pa ramagnetic detector to produce an electrical signal, which is linearly proportional to the O2/CO2 concentrations.



### 12.3 Hydrogen Chloride (Table 1.1 Compound List) Hydrogen chloride is determined following pro cedures outlined in EPA Reference Method 26A.

Sampling Equipment and Procedures Figure 12-3-1 presents a schematic of the sampling train. The empty first impinger in the figure is optional. The nozzle and heated probe is constructed of borosilicate glas s and connected to a heated filter holder containing a
Teflon ® coated quartz filter. This is connected to an impinger train. The first and second impingers are each charged with 100 mL of 0.1 N H 2 SO 4 . The third and fourth impingers cont ain 100 mL of 0.1 N NaOH. The fifth impinger is charged with 200-300 grams of indicating silica gel. All impingers are maintained in a crushed ice bath. A gas measuring control console with a leakless vacuum pump, a calibrated dry gas meter, a calibrated orifice, and inclined manometers are connected to the final impinger via an umbilical cord to complete the train.

Flue gas velocity is measured with a calibrated S-type pi tot tube (provided with extensions) fastened alongside the sampling nozzle. Flue gas temperature is monitored with a calibrated direct readout pyrometer equipped with a chromel-alumel (Type K) thermocouple positioned near the sampling nozzle. The impinger exit gas temperature
is monitored with a calibrated direct readout pyrometer equipped with Ty pe K thermocouples positioned in the sample gas stream after the last impinger. Stack gas st ream composition (carbon dioxi de and oxygen content) is determined as described previously. The sampling rate is adjusted, based on stack velocity, at each point to ensure the sample is collected isokinetically.

After completion of the sample run, the sample train is leak checked. Following a successful leak check, the contents of the first and second imping ers are measured and transferred to a borosilicate glass sample container
with a Teflon ® lined lid. The impingers are then rinsed with deionized water into the same sample container.

Sample Analysis The samples are analyzed for chloride using ion chromatography (IC) as described in the Method 26A. All IC is performed using acceptable laboratory procedures. Adhe rence to prescribed quality control procedures as described below ensures data of consistent and measurable quality. Analytical quality control focuses on instrument calibration as pe r EPA Reference Method 26A and the use of control standards to provide a measure of analytical precision and accuracy. Sp ecific acceptance criteria is defined for analytical operations including calibrations and control standard analyses.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 29 of 66Figure12‐3‐1EPAReferenceMethod26AHydrogenChlorideSamplingTrainOptionalTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 30 of 66 Analytical quality control includes analysis of a laboratory blank, method spikes, and duplicates. The laboratory
blank consists of the DI H 2 O used for any sample dilutions analyzed per the procedures specified in draft Method 26A to check for laboratory contamination. Method spikes for EPA Reference Method 26A are prepared by spiking a representative amount of HCl into 0.1 N H 2 SO 4 and adjusting the volume to 100 mL using DI H 2 O. The method spikes are handled in the same manne r as (and analyzed wi th) the field samples.

Data Acquisition and Reduction Data is recorded at the time of collection on preprinted data sheets. Calculations are performed (where possible) with preprogrammed calculators or spreadsheet software.

Quality Control Calibration and leak checking of the appropriate samplin g equipment, including meter boxes, temperature sensors, nozzles, pitot tubes, and umbilical s, are performed according to th e requirements specified in EPA ’ s “ Quality
Assurance Handbook, Volume III ” (600/4-77-027b). The results are documented and retained.

Dry gas meters are calibrated before and after sampling. Thermocouples are calibrated against mercury thermometers, and aneroid barometers are calibrated against a mercury barometer. The temperature of the gas leaving the impinger train is kept at 68 ° F or less throughout the sampling by maintaining the ice bath. Care is taken to prevent sample loss during sample recovery. Sample storage bottles are purchased new or cleaned prior to use and are kept sealed at all times. Samples are transported to the laboratory under chain-of-custody. Upon receipt by the laboratory, the liquid level in each sample bottle is noted. If a noticeable amount of liquid has been lost, the sample is voided. Reagents used during testing meet American Chemical Society specifications. A blank is analyzed with each series of samples.

Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. Calculations are verified by a second person.



### 12.4 Formaldehyde, Methanol and Ethylene Glycol (Table 1.5 Compound List) Formaldehyde, methanol, and ethylene glycol are dete rmined following procedures outlined in EPA Reference Method 316 and through a series of analysis developed by Enthalpy Analytical, Inc. to meet the objectives of
the PVC ICR.

Sampling Equipment and Procedures

Figure 12-4-1 presents a schematic of the sampling tr ain. The nozzle and heated probe is constructed of borosilicate glass and is connected to an impinger train. When stack moisture levels are high, the first impinger is left empty. The second, third and four th impingers are each charged with 1 00 mL of distilled water. The fifth impinger is charged with 200-300 gram s of indicating silica ge l. All impingers are maintained in a crushed ice bath. A gas measuring control console with a leakless vacuum pump, a calibrated dry gas meter, a calibrated orifice, and inclined manometers are connected to the final impinger via an umbilical cord to complete the train.

Flue gas velocity is measured with a calibrated S-type pi tot tube (provided with extensions) fastened alongside the sampling nozzle. Flue gas temperature is monitored with a calibrated direct readout pyrometer equipped with a chromel-alumel (Type K) thermocouple positioned near the sampling nozzle. The impinger exit gas temperature is monitored with a calibrated direct readout pyrometer eq uipped with Type K thermocouples positioned in the sample gas stream after the last im pinger. Stack gas stream composition (carbon dioxide and oxygen content) isTest Plan for EPA ICR – Shintech Louisiana LLC

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After completion of the sample run, the sample train is leak checked. Following a successful leak check, the contents of the first, second and third impingers are measured and transferred to a polyethylene sample container. The contents of the fourth impinger are measured and transferred to a separate polyethylene sample container. The impingers are then rinsed with deionized water into the respective sample containers.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 32 of 66Figure12‐4‐1EPAReferenceMethod316SamplingTrainTest Plan for EPA ICR – Shintech Louisiana LLC

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FormaldehydeThe samples are analyzed for formaldehyde using ion chromatography (IC) as described in the Method 316. All IC is performed usin g acceptable laboratory procedures. Adhe rence to prescribed quality control procedures as described below ensures data of consistent and measurable quality. Analytical quality control focuses on instrument calibration as per EPA Reference Me thod 316 and the use of control standards to provide a measure of analytical precision and accuracy. Specific acc eptance criteria are defined for analytical operations including calibrations and c ontrol standard analyses.

Analytical quality control includes analysis of a laboratory blank, method spikes, and duplicates. The laboratory
blank consists of the DI H 2 O used for any sample dilutions analyzed per the procedures specified in Method 316 to check for laboratory contamination. Method spikes for EPA Reference Method 316 are prepared by spiking a representative amount of formaldehyde into DI H 2 O. The method spikes are handled in the same manner as (and analyzed with) the field samples.

An EPA Method 316 blank train (identical to the source sample train) is setup with one of the test runs. The blank train samples along with a blank DI H 2 O site blank is analyzed with the source samples.

An analysis of the final impinger is performed separately to evaluate sample train collection efficiency.

MethanolMethanol is analyzed from the Method 316 impingers using a modified Method 308 approach. An analysis of the final impinger is performed separately to evaluate sample train collection efficiency by GC/FID.

A matrix spike (MS) is prepared and analyzed for each source.

Ethylene GlycolEthylene glycol analysis is conducted from the Meth od 316 impingers using a modification of EPA Method 18 which employs an azeotropic distillation to remove water from the sample to ensure complete derivatization. An analysis of the final impinger is performed separately to evaluate sample train collection efficiency. An internal standard and surrogate are added to ensure accurate results. Enthalpy has developed this method due to the known challenges analyzing ethylene glycol at low concen trations from a water matr ix by GC/FID. A matrix spike (MS) is prepared and analyzed for each source.

Data Acquisition and Reduction

Data is recorded at the time of collection on preprinted data sheets. Calculations ar e performed (where possible) with preprogrammed calculators or spreadsheet software.

Quality Control

Calibration and leak checking of the appropriate samplin g equipment, including meter boxes, temperature sensors, nozzles, pitot tubes, and umbilicals, are performed according to the require ments specified in EPA’s “Quality Assurance Handbook, Volume III” (600/4-77-027b). The results are documented and retained.Test Plan for EPA ICR – Shintech Louisiana LLC

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Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. Calculations are verified by a second person.



### 12.5 Semivolatile Orga nic Compounds (Table 1.4 Compo und List, Site Specific HAP) The semivolatile organic compounds train is described in SW-846 as Method 0010. Semivolatile organic compound analysis is conducted according to EPA SW-846 8270D.

Sampling Equipment and Procedures

The Method 0010 Sampling Train is shown in Figure 12-5 -1. Please note that an optional extra impinger is depicted before the silica gel impinger. The impinger train is assembled in the sample recovery area. The pre-cleaned impingers are assembled with the first impinger being an empty knockout impinger with a short stem. The purpose of this impinger is to collect the majority of the condensate which forms in the condenser coil and XAD resin module. The next two impi ngers are standard type Greenberg-Smi th impingers, each containing 100 mL of HPLC grade water. The fourth impinger is empty and the fifth impinger is ch arged with approximately 300 grams of indicating silica gel. The glass fiber filt er is placed in a filter holder and connected to the
condenser coil and XAD resi n module. The train components are then transferred to the sampling location and assembled completely.

After the sampling train is assembled and all components are heated appropriately, a leak check is performed. During sampling, the temperature of the so rbent module resin is not to exceed 68 ° F. The probe temperature is
maintained above 248 °F + 25 °F ; the f ilter temperature is controlled at 248 ° F + 25 ° F, and the outlet of the silica gel impinger is maintained at less than 68 ° F during operation.

The sampling train is leak-checked at the beginning and en d of the run and each port change. An acceptable leak rate is less than 0.02 acfm at the highest vacuum measured plus one inch of Hg or less than 1.5% of the sampling

rate.

After a successful pre-test leak check, the train assemb ly is placed in the stack and operated along each of the traverse points for each of the two horizontal traverses. Sampling is performed for a total of three hours using a sampling rate between 0.5 and 0.75 scfm to collect a total sample volume of at least 106 dscf (3 dscm). Sampling
train data are recorded on standard data forms.

The Method 0010 sampling trains are recovered followi ng the scheme presented in Figure 12.5.2. Liquid samples are placed in pre-cleaned amber glass sample containers with Teflon ® liners. The filters are placed in pre-cleaned glass petri dishes or amber glass sample containers. The reagent blank containers for the train
fractions are listed in Table 12-5-1.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 35 of 66Figure12‐5‐1M0010EPAMethodSamplingTrainforSemivolatileOrganicsTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 36 of 66 Figure 12-5-2 Sample Recovery Pro cedures for Method 0010 Sampling TrainsTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 37 of 66 Reagent blank samples are collected as follows:

Table 12-5-1 – M0010 Reagent Blank Samples

Reagent Amount Fraction Blank Trains Trip
Blanks

HPLC Water 300 mL IMP CON 1/source 1/trip

Methanol/Methylene
Chloride 200 mL FHR, BHR

IMPR 1/source 1/trip

XAD Sorbent Module a N/A ---- 1/source 1/trip

Glass Fiber Filter N/A ---- 1/source 1/trip

Methanol 200 mL ---- 1/source -----

Methylene Chloride 200 mL ---- 1/source -----

a XAD sorbent module is randomly selected from the on-site XAD modules used for the test program.

Sample Analysis

Semivolatile Organic Compounds

The M0010 semi-volatile samples are normally analyzed according to SW-846 Method 8270D. For the PVC ICR, the EPA mandates that SW-846 Method 3542 be used for sample preparation and SW-846 Method 8270D with a low resolution GC/MS SIM analytical finish be used for analysis. The methanol/methylene chloride front half (FH) probe rinse is concentrated to about 2 mL using a Kuderna-Danish (KD) appa ratus and then combined with the filter in a soxhlet apparatus. A set of 8 Base/Neutral/Acid (BNA) surrogates along with the above labeled standards is spiked into the soxhlet at 100 mg leve ls. The combined filter and FH rinses are then soxhlet extracted with methylene chloride for 16 hours.

The methanol/methylene chloride back half rinses (BHR ) are concentrated to about 2 mL using a KD apparatus and then combined with the XAD resin in a soxhlet appa ratus. The eight BNA surroga tes along with the labeled standards are spiked into the soxhlet and the combined XAD and BHR are soxhlet extracted with methylene
chloride for 16 hours.

The impinger water is spiked with the eight BNA surrog ates and labeled standards at 100 mg levels and then liquid-liquid extracted with methylene chloride.

Each extract is dried over sodium sulfate, concentrated to a volume of 5 mL and cleaned using gel permeation chromatography (GPC).

For a list of the compounds that will be determined dur ing this test program by SW-846 Method 0010, please
refer to Table 5.1.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 38 of 66 Data Acquisition and Reduction

Data will be recorded at the time of collection on preprinted data sheets. Calculations will be performed (where possible) with veri fied preprogrammed calculators or spreadsheet software.

Quality Control

The standard M0010 pre-cleanup requirements include se veral unique preparation steps which ensure that the sampling train components are not c ontaminated with organic compounds that may interfere with the analysis. The glassware, glass fiber filters, and XAD adsorbing resin are pre-cleaned using strict protocols.

The glassware is normally cleaned as shown in Table 12-5-2. Glassware is washed in soapy water, rinsed with distilled water, baked and then rinsed with acetone followed by methylene chloride. Once the glassware is dried, the open ends will be sealed with either methylene chloride-rinsed aluminum foil or Teflon ® tape.

Non-glass components (such as the Teflon ® filter supports and se als, tweezers, Teflon ® squeeze bottles, nylon nozzle, and probe brushes) are cleaned following the same procedure, except that no baking is performed.

Table 12-5-2 Organic Glassware Cleaning Procedure (Train Components, Sample Contai ners, and Laboratory Glassware) NOTE: USE VITON GLOVES AND ADEQUATE VENTILATION WHEN RINSING WITH
SOLVENTS
1. Soak all glassware in hot soapy water (AlconoxÔ).

2. Tap water rinse to remove soap.

3. Deionized H2O rinse (x3). a

4. Bake at 450° for 2 hours. b

5. Methanol rinse (x3), (pesticide grade).

6. Methylene chloride (x3), (pesticide grade).

7. Cap glassware with Teflon ® tape or methylene chloride rinsed aluminum foil.

8. Mark cleaned glassware with color-coded identification sticker.

a (x3) = three times.

b Step (4) is added to the cleanup procedure to replace th e dichromate soak specified in the reference method. It has been demonstrated that baking at 450 °F sufficientl y removes organic artifacts. It is not used for probe liners and non-glass components of the train that cannot withstand 450 °F (i.e., Teflon ® -coated filter screen and seals, tweezers, Teflon ® squeeze bottles, nylon probe and nozzle brushes).Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 39 of 66 The XAD adsorbent resin and glass fiber filters are pre-cleaned by separate procedures. The XAD, which is purchased in 100 gram amber glass containers, is placed in the glass modules under st rict laboratory-controlled
conditions. Each lot of XAD resin is recorded in a laboratory notebook and a control sample is withdrawn for a quality assurance analysis. The laborato ry archives a sample from each lot for analysis with the field sample as a
lab blank.

To prepare the filters, a batch of 50 filters are placed in a soxhlet extr action apparatus and extracted using methylene chloride for 16 hours. Afterwards, the filters are checked for holes, tears, creases, and discoloration. Acceptable filters are placed in pre-cleaned containers a nd labeled by date of extraction and sealed with Teflon ® tape.

The remaining equipment preparation in cludes routine checking and calibra tion of the Method 5-type equipment as specified in Method 0010.

During one of the runs, an M0010 field blank train is a ssembled with glassware that has previously been use for M0010 sampling. This train is charge d exactly as the other M0010 trains and left at a sampling location during
the test run. The field blan k train is then recovered with the other M 0010 train for that run. The sample train
results are used to assess the level of contamination that occurs from handling, charging, recovering, and transporting the sampling train.

One sample train blank is prepared for each source. One se t of trip blanks are collected and archived for future examination, if contam ination is determined. A lab method blank using the control XAD blank that is withheld during the XAD module preparation phase is also analyzed.

QC guidelines can be found in SW-846 Method 0010.

To further ensure sample integrity and stability, smoking is not allowed in or around the Laboratory Recovery Area, and XAD resin samples are immediately stored at or below 4 °C.

Data transfers are minimized. Field and laboratory data sheets are checked for completeness and accuracy. Calculations are verified by a second person.



### 12.6 Total Hydrocarbon Concentrations (Table 1.1 Compound List, 30-Day Monitoring) Total hydrocarbon (THC) concentrations are sampled using EPA Reference Method 25A and analyzed by WESTON on site with a flame ionization detector (FID ) analyzer. It should be noted that Method 25A determines total organics, includin g methane, which is not a regulated volatile organic compound (VOC).

Sampling Equipment and Procedures

Figure 12-6-1 is a schematic of the EPA Reference Met hod 25A sampling system. An extractive system is used at the sampling locations to obtain ve nt gas samples. Samples are withdr awn continuously at a single point and transported to the FID through a heated probe Teflon ® filter, and heated Teflon ® sample line. All hydrocarbon measurements are made on a "hot, wet" basis.

Sample Analysis

A continuous emission monitor is used to measure the to tal hydrocarbon concentration in the source gas. This analyzer utilizes a FID as described by EPA Reference Method 25A. The technique is not selective between species, and the results are reported as carbon volume equiva lents of the calibration gas (propane in nitrogen or propane in air).Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 40 of 66 Calibration gases are introduced at the probe and recove red through the sampling and analytical system. After zeroing, a high level certified calibration gas is used to span the analyzer and generate a linear response line between the zero and high gas concentration. A low and mid-level certified calibration gas is then introduced to the analyzer to verify the linear response of the analyzer. An interference response study was performed by the manufacturer of the analyzer. The data from this study are on file at WESTON.

Data Acquisition and Reduction

Data is acquired electronically using a computer with software designed by WESTON for EPA Reference Method 25A analysis.

Quality Control

The calibration and check gases are propane, in either ni trogen or air, certified ac cording to EPA Protocol-1. Following each sample run, the calibration drift of the sy stem is checked by introducing the zero and one upscale gas to the system and recording the response. This differ ence in concentration must be within three percent of the full scale span value.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 41 of 66Figure12‐6‐1EPAReferenceMethod25ASamplingTrainTest Plan for EPA ICR – Shintech Louisiana LLC

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### 12.7 Volatile Organic Compounds (SW8 46 Method 0031) (Table 1.3 Compound List) Volatile organic compounds are measured using the Volatile Organic Sampling Train (VOST). Four runs of SW-846 Method 0031 are conducted on each stack. Analysis is performed by Maxxam Analytics, Inc. using a gas chromatograph with a mass spectrophotometer (GC/ MS) according to the procedures outlined in SW-846
Method 8260B.

VOST Sampling Equipment and Preparation

The volatile organic sampling train (VOST) of SW-846 Me thod 0031 is used to collect the volatile organic samples. Figure 12-7-1 is a schematic of the Method 0031 sampling train.

The VOST equipment, except the sorbent cartridge, is cleaned and calibrated by WESTON according to Method 0031. The sorbent cartridges used for sampling are prepared by an outs ide lab. This consists of first cleaning the glass tubes and metal parts with a nonionic dete rgent, rinsing in organic-free water, and drying at the specified temperatures. The Tenax and Anasorb ar e soxhlet extracted with methanol and dried. The
Tenax and Anasorb tubes are then assembl ed and conditioned by heating to 190 ° C while organic-free nitrogen is passed through them. Each set of tub es are blank checked by thermal desorption and gas chromatographic techniques prior to sampling to ensure cleanliness.

VOST Sampling Procedures

The volatile organic sampling train is assembled as shown in Figure 12-7-1. Samples are collected using a set of paired Tenax (two) and Anasorb cartridges, with each cartridge preceded by a condensing module. The first condenser cools the gas stream and condenses th e water vapor present. The flue gas and condensed moisture then pass through a pair of cartridges cont aining 1.5 grams of Tenax resin (60-80 mesh). The condensate is collected in an impinger that is continually purged by the gas stream.

The second condenser and cartridge containing Anaso rb serves as a backup for breakthrough compounds. Following the third cartridge is a silica gel dr ying tube for residual moisture removal.

Each sample run consists of four or five tube sets. The individual tube sets are collected at a set sample volume for at least 20 minutes. The sample volumes for each of the sets of cartridges are approximately 20 liters. Sampling is conducted at a single point. The system is leak-checked by closing the valve at the inlet to the first condenser and evacuating the system at 10 inches Hg. The system will then be isolated and the leak
rate noted. The leak rate must be less than 1 inch Hg after one minute. The train will be returned to atmospheric pressure by purging through a charcoal tube . The leak checks will be conducted before and after
each set of VOST tubes is collected. The first three tube sets will be analyzed. The fourth tube set will be
archived. A fifth set will be retained as a field blank.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 43 of 66 Figure 12-7-1 EPA Method 0031 Volatile Orga nic Sampling Train (VOST)Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 44 of 66 Gas sample temperatures are to be monitored at the outle t of the sampling probe and the inlet to the Tenax and Anasorb cartridges using thermocouples. The temperature of the gas through th e sorbent tubes is maintained at
less than 20 °C.

VOST Sample Recovery

After recovering the sample for the VOST the system is leak-checked as required, the cartridges are capped and placed in original glass culture tubes with glass w ool to absorb the shock. The volume of condensate impinger is measured in a precleaned graduated cylinde r and transferred to 40 mL VOA vials and diluted to volume with HPLC water to decrease headspace, whic h reduces the possibility of revolatilization of the compounds. To reduce reactivity store samples at 4  C.

The samples collected during each VOST run consist of th e four sets of sorbent tubes (Tenax cartridge, Tenax cartridge, and Anasorb cartridge), and the condensate. One additional set of Tenax, Tenax, and Anasorb cartridges serves as field blanks per day. The set is ta ken to the sampling site and the end caps removed for the period of time required to exchange one set of tr aps on the VOST. After the VOST traps have been exchanged, the end caps are replaced on the field blanks, and are stored and analyzed with the field samples.

A second set of blank cartridges is included in the cartri dge shipment to the test site. These trip blanks are treated like the other cartridges except that the end caps are not removed dur ing storage at the site. These are also analyzed with the field samples.

One pair of blank cartridges, a laboratory blank, remains st ored in the laboratory. This blank is analyzed if the field or trip blanks show hi gh contaminant concentrations.

VOST Sample Analysis

The volatile organic contents of each cartridge and co ndensate sample are therma lly desorbed onto a gas chromatographic column (GC). The Tenax cartridges are analyzed separately from the Anasorb cartridge;
likewise the condensate fractions are al so analyzed separately. Prior to sample recovery, the contents of the sorbent cartridges are spiked with a deuterated standard as well as other unl abeled internal standards that are similar to the analytical character istics of the compounds of interest. Following spiking, the cartridge contents are thermally desorbed usin g an inert gas which is then bubbled through organic-free water. The desorbed components pass into the bo ttom of the water column where they are purged from the water, and collected on an adsorbent trap. After completion of the desorption, the com pounds are described from the adsorbent trap onto a gas chromatographic column.

For the condensate sample, the sample fraction is spiked with the same internal standards indicated above. Afterward, an inert gas is bubbled through the solution at ambient temperature and the volatile compounds are transferred from the aqueous phase to the vapor phase. The vapor is swept through a sorbent column where the volatile compounds are trapped. Upon completion of purging, the sorbent column is heated and backflushed with inert gas to desorb the components onto a gas chromatographic column.

The volatile organic target compounds of interest are analyzed following the procedures specified in EPA
Reference Methods 5041A for the media and 8260B for the condensate.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 45 of 66 Following the procedures outlined in Method 8260B, th e volatile compounds are directed into the GC/MS system. The volatile compounds are separated by temp erature programmed gas chromatography and detected by low-resolution mass spectrometry. The concentrations of the volatile compounds of interest are calculated using the labeled and unlabeled internal standard technique.

For a list of the compounds that will be determined dur ing this test program by SW-846 Method 0031, please
refer to Table 5.1.

Volatile Sample Quantitative Analysis

Quantitative analysis is performed by GC/MS using extracted ion current profile (EICP) areas:

The GC/MS system is calibrated using a quantitation i on and the compound concentra tion is determined using an internal standard technique.

For compounds where standards are not available, co mpound concentrations are determined using known response factors from the closest internal standard.

Volatile Analysis Quality Control

The major QC procedures contained within the met hod will include GC/MS tuning, calibrations system performance checks and analysis of specific QC check sa mples. During actual sample measurements, several field blanks, trip blanks and a laboratory method blank are analyzed with the field samples. The quality of the analysis is assured through reproducible calibration and testing of the purge and trap and GC/MS systems.

Spiked cartridges are transported to th e field, and returned to the laborator y and analyzed to determine analyte recovery from the sorbents.

VOST Sampling QC Procedures

Quality Control procedures for VOST sampling are designed to ensure the collection of high quality gas stream
concentrations and emission data w ithout interference of contaminants. Gas stream concentrations of each analyte are determined by dividing the mass of each analyte collected by th e standardized gas volume
collected.

VOST sampling QC procedures include:

 Use of precleaned glassware.

 Sampling train composed of glass and/or Teflon.

 Sorbent traps are prepared and stored in a manner to prevent contamination.

 Recovery procedures are completed in a clean environment.

 Four samples are collected and three are analyzed per run to ensure adequate analysis.

 Samples are stored and shipped at reduced temperature (~4 °C).

 At least one field blank per day and one trip blank per test program will obtained and analyzed.Test Plan for EPA ICR – Shintech Louisiana LLC

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Data quality audits are conducted usi ng data quality indicators which require the detailed review of: (1) the recording and transfer of raw data; (2) data calcula tions; (3) the documentation of procedures; and (4) the selection of appropriate data quality indicators.

Some of the data quality indicators to be used for data validation are:

 Comparison of the relative concentrations of th e emissions at the different sampling locations.

 Comparison of the results for a particular parame ter with those from each condition (i.e., are the concentrations similar and do they show the same relationship for a material balance).

 All data and/or calculations for flow rates, moisture content, and isokinetic rates made using a computer software program are validated by an independent chec k. All calculations are spot checked for accuracy and completeness.

In general, all measurement data is validated based on the following criteria:

 Process conditions during sampling or testing,

 Acceptable sample collection procedures,

 Consistency with expected other results, and

 Adherence to prescribed QC procedures. Any suspect data is flagged and identified according to the specific deviation from prescribed criteria and its potential effect on the data quality. Upon completion of testing, the field coordinator is responsible for preparation of a data summary including calculation results and raw data sheets.

The test report includes QA/QC summaries reporting the QC data collected and the results of any audits. The outside laboratory reports its QA/QC results in the an alytical report. All QA/QC results are reviewed internally by WESTON before the data are released; any data that fail to meet the program’s QA requirements
are noted.



### 12.8 Speciated HAP – Direct Interface (Table 1.1 Compound List, Site Specific HAP) EPA Method 18 outlines three different sampling appro aches with gas chromatogr aphy as the analytical method. The three approaches include direct interface, adsorption media, or whole gas sample collection utilizing flexible Tedlar® bag enclosures. The GC conditions are not defined as the number of compounds and compound mixtures requires selective GC conditions.

Sampling Equipment and Procedures

For the direct interface approach, the sampling equipm ent incorporates a heated sample probe with filter (in-stack or heated-out-of-stack), heated sample line, heated diaphragm pump. The sample is delivered continuously to the onsite mobile laboratory at a rate of 1-2 L/min. Excess sample gas is vented from the laboratory.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 47 of 66 At all times during the sampling period, the heated samp ling system is maintained at a temperature above the condensation temperature of the stack. Maintaining th e sample above the condensation temperature ensures that the target compounds are maintained in the vapo r phase and any moisture present in the sample is not condensed (condensed moisture will selec tively remove polar organic compounds).

A schematic representation of the direct interface samp ling and analytical equipm ent is shown in Figure
12-8-1.Test Plan for EPA ICR – Shintech Louisiana LLC

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### Sample Analysis

For the analysis of gaseous samples, the chromatography conditions required to resolve and quantify the target compounds are developed prior to sample collection.

The analytical system is comprised of three main components, sample introduction system, chromatograph with selected columns and detector, and the da ta collection system with report generator.

The sample injection system uses a he ated rotary valve with Teflon® sample loop. The certified calibration gas mixtures and samples are introduced to the chromat ograph using the same inject or. The GC uses capillary columns which are commercially available and chosen to resolve the target compounds within a reasonable time frame, 5 - 45 minutes.

Detection and relative intensity of calibration gas or samp le gas matrices is performed by the GC FID detector, which measures a change in potential across an enclo sed flame. The difference in potential is directly proportional to the concentration present. Calibration curves for the target compounds are prepared at a minimum of three concentration levels, and brack et the concentration range of the samples.

The identity of target compounds is determined by comp arison of the sample gas retention times compared to the retention times of calibration gas mixtures. The con centration of the target compounds is determined from comparison of the intensity of the sample peaks comp ared to the intensity of the calibration peaks.

Commercially available calibration gas mixtures are obtained which meet the method accuracy criteria.

For high concentration sources, where commercially ava ilable gas standards are not available, calibration gas mixtures are prepared by injection of a known mass of the target compound into a known volume of air or nitrogen.

For a list of the compounds that will be determined duri ng this test program by EP A Method 18, please refer to
Table 5.1.



### Data Acquisition and Reduction

The output from the GC/FID system is collected usi ng a commercially available data acquisition interface and software. The system generates the calibration cu rves and produces a report and chromatogram at the conclusion of each analysis.



### Quality Control

Quality controls for the direct interface system include a leak check of the entire sampling system and target compound recovery checks.

For the direct interface recovery study, the mid-level ca libration gas (for at least one of the target compounds) is presented to the sample probe. The calibration gas is collected and analyzed as a sample. An acceptable recovery yields a GC response to within 10% of the direct calibration standard analyzed response.Test Plan for EPA ICR – Shintech Louisiana LLC

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### 13. Laboratory Sample Summary Table 13-1 Sample Collection Summary, Main ICR Test Program

Container Number Number
Collected /Test Program Designation (1) Description

EPA M26A

– HCl (ICR Table 1.1 Compound List)

1 0 ‐ Filter

2 0 ‐ Front Half (FH) Rinse

3 3 S Knockout/Acid Impingers

4 0 ‐ Alkaline Impingers

5 0 ‐ Silica Gel

6 1 RgB 0.1 N H2SO4 Diluted w/ Water

7 0 ‐ 0.1 N NaOH

8 1 RgB Rinse Water

9 1 RgB Acetone
HCl is collected with a M26A isokinetic sampling train consisting of sulfuric acid (H2SO4) charged impingers.
The samples are analyzed using IC by Enthalpy Analytical. This approach has an in

‐ stack MDL of < 15ppb / analyte based on a minimum sampling volume of 2.0 DSCM. Samples will be recovered into HDPE bottles.

As this test program is not to demonstrate initial compliance, audit samples have not been requested.

‐ One fraction analysis per train ‐ EPA M316

– Formaldehyde, Methanol, Ethylene Glycol (ICR Table 1.5 Compound List)

1A 4 3S, 1FB FH Rinse, Knockout, Imp. 1, Imp.2

1B 4 3S, 1FB Imp. 3

2 1 RgB Reagent Water

3 0 ‐ Silica Gel
Flue gas is withdrawn isokinetically from the source and formaldehyde, methanol, and ethylene glycol is
collected using an initial condenser followed by three impingers charged with high purity water. The
condenser catch will be combined with the contents of the first two impingers and the third impinger will
be recovered separately to evaluate the train for breakthrough. Formaldehyde Formaldehyde will be analyzed by Enthalpy using the modified pararosaniline method. Formaldehyde

reacts with the acidic pararosaniline and sodium sulfite to form a purple chromophore that is measured by spectrophometer at 570nm. The MDL for formaldehyde is 0.05  g/mL. A matrix spike (MS) will be prepared and analyzed for each source.

‐ Two fraction analyses per train ‐ Methanol
Methanol is analyzed by Enthalpy from the Method 316 impingers using a modified Method 308 approach
with analytical MDL of 0.50  g/mL. A matrix spike (MS) will be prepared and analyzed for each source.

‐ Two fraction analyses per train ‐ Ethylene Glycol Ethylene glycol analysis will be performed by Enthalpy from the Method 316 impingers using a modification
of EPA Method 18 which employs an azeotropic distillation to remove water from the sample to ensure a complete derivatization. An internal standard and surrogate are added to ensure accurate results. Enthalpy has developed this method due to the known challenges analyzing ethylene glycol at low

concentrations from a water matrix by GC/FID with a 0.50  g/mL analytical MDL. A matrix spike (MS) will
be prepared and analyzed for each source.

‐ Two fraction analyses per train ‐Test Plan for EPA ICR – Shintech Louisiana LLC

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‐ 846 0010/8270D

– Semi

‐ VOHAPs (ICR Table 1.4, Speciated HAP Compound List)

1 5 3S, 1FB, 1RgB Filter

2A 4 3S, 1FB Probe / FH Rinse

2B 1 RgB FH Rinse Blank

3 5 3S, 1FB, 1RgB Sorbent Trap

4 4 3S, 1FB Condensate and BH Filter House

5 4 3S, 1FB Filter to 1 st Wet Impinger

6 0 ‐ Silica Gel

7 1 RgB Water

8 1 RgB MeOH

9 1 RgB MeCl 2 Semi

‐ VOHAPs are collected by EPA SW

‐ 846 Method 0010 utilizing a Method 5 type configuration with the
addition of an XAD trap after the heated filter. Enthalpy packs and spikes ball and socket traps with blank
checked XAD

‐ 2 resin. After collection the filter, XAD trap, rinses, and water are recovered and returned to Enthalpy for analysis. Samples are prepared by SW

‐ 846 Method 3542 and analyzed by EPA SW

‐ 846
Method 8270D with a low resolutions GC/MS SIM analytical finish. The analytical technique has an MDL of <0.05 ppb/compound in

‐ stack based on a sampling volume of 3 DSCM

‐ Three fraction analyses per train ‐ SW

‐ 846 Method 0031/5041/8260B

– VOC by VOST (ICR Table 1.3 Compound List)

1 3 S Tube Set

– Tenax/Tenax/Anasorb

2 3 FB Tube Set

– Field Blank (1/Test Run)

3 1 TB Tube Set

– Travel Blank (1/Test)

4 3 S Condensate

5 3 FB Condensate

– Field Blank Sample is collected by SW

‐ 846 M0031, samples are prepared by SW

‐ 846 5041, and samples are analyzed by

SW

‐ 846 8260B. Analysis will be performed by Maxxam Analytics. Samples will be collected at 1L/min

over two hours, with tube sets being changed every twenty minutes. Each tube set consists of two Tenax
tubes and one Anasorb tube. Six tube sets, one condensate, one field blank tube set, and one field blank
condensate will be captured per test run. Traps for each test run will be combined to lower detection
limits.

‐ Three fractions per analyses ‐ (1) 

### S=Sample, FB=Field Blank, RgB=Reagent Blank, TB=Trip BlankTest Plan for EPA ICR – Shintech Louisiana LLC

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### 14. VOST Detection LimitsNONT,

French Test Name : Test Code : AIR

VOCVOSTM-A

Spanish Test Name : Description :

Instrument :
Result Unit : Storage Temp :
Preservation Code : Default Report On ? :

Current :

English Method :
French Method : Spanish Method :

Test Sig. Digits : DL Sig. Digits :
Linked Tests :
Test Location : Matrix Code :
SubMatrix Code :
Location Code : Report Group Code :

Detector : Parameter Group : Analysis Time : Department No :

Product Code :

Reference Number : Aliquot Volume : VOST Analysis (5041mod) Analyse VOST (5041mod) VOST Analysis (5041mod) VOST Analysis

GC

ug
4

YES

Yes

EPA 5041mod(M0030) EPA 5041mod(M0030) EPA 5041mod(M0030)

3

2 BRL SOP-00302 VOLAIR 4014 14 VOL MS VOC NONT English Test Name :

Calculation Block : NO Test Group : VOLVOS

Price Bin # : 330.00

_______________________________________ 1


## List of Parameters

Code Parameter Description Rpt. Def. Prm. Grp. Rpt. Ord. RDL IDL Instr. Ord.

0

0 105 BN NO Hexachlorobutadiene BASEN8

0 0.011 35 CB YES Chlorobenzene CB1

0 0.02 44 CB YES 1,3-Dichlorobenzene CB2

0 0.02 45 CB YES 1,4-Dichlorobenzene CB3

0 0.02 46 CB YES 1,2-Dichlorobenzene CB4

0 0 103 CB NO 1,2-Dichlorotetrafluoroethane CB41

0 0 104 CB NO 1,2,4-Trichlorobenzene CB6

0 0.015 9 VOL YES Iodomethane HAL 43

0.015 2 VOL YES Chloromethane HAL1

0 0.01 15 VOL YES cis-1,2-Dichloroethylene HAL10

0.011 16 VOL YES Chloroform HAL11

0 0.014 19 VOL YES 1,1,1-Trichloroethane HAL12

0 0.016 20 VOL YES Carbon Tetrachloride HAL14

0 0.007 17 VOL YES 1,2-Dichloroethane HAL15

0 0.011 24 VOL YES Trichloroethylene HAL16

0 0.011 23 VOL YES 1,2-Dichloropropane HAL17

0 0.011 26 VOL YES Bromodichloromethane HAL18

0 0.013 3 VOL YES Vinyl Chloride HAL2

0 0.01 27 VOL YES cis-1,3-Dichloropropene HAL20

0 0.007 28 VOL YES trans-1,3-Dichloropropene HAL21

Page 1 of 20 0.016 22 VOL YES 1,1,2-Trichloroethane HAL22

0 0.018 34 VOL YES Tetrachloroethylene HAL23

0 0.009 29 VOL YES Dibromochloromethane HAL24

0 0.014 41 VOL YES Bromoform HAL26

0 0.014 42 VOL YES 1,1,2,2-Tetrachloroethane HAL27

0 0.02 1 VOL YES Dichlorodifluoromethane (FREON 12) HAL28

0 0.015 4 VOL YES Bromomethane HAL3

0 0.009 5 VOL YES Chloroethane HAL4

0 0.01 6 VOL YES Trichlorofluoromethane (FREON 11) HAL5

0 0.011 8 VOL YES 1,1-Dichloroethylene HAL6

0 0.019 11 VOL YES Methylene Chloride(Dichloromethane) HAL7

0 0.01 14 VOL YES trans-1,2-Dichloroethylene HAL8

0 0.012 12 VOL YES 1,1-Dichloroethane HAL9

0 0.015 38 VOL YES m / p-Xylene MAH 16

0 0.009 21 VOL YES Benzene MAH1

0 0.014 32 VOL YES Toluene MAH2

0 0.014 37 VOL YES Ethylbenzene MAH3

0 0.015 40 VOL YES o-Xylene MAH4

0 0.012 39 VOL YES Styrene MAH7

0 0.045 7 VOL YES Acetone (2-Propanone) VOL1

0 0.026 10 VOL YES Carbon Disulfide VOL3

0 0 102 VOL NO 1,2,4-Trimethylbenzene VOL41

0 0 101 VOL NO 1,3,5-Trimethylbenzene VOL57

0 0.019 30 VOL YES Methyl Isobutyl Ketone VOL6

0 0.031 31 VOL YES Methyl Butyl Ketone (2-Hexanone) VOL60

0 0.01 33 VOL YES Ethylene Dibromide VOL62

0 0 100 VOL NO Trichlorotrifluoroethane VOL67

0 0.036 18 VOL YES Methyl Ethyl Ketone (2-Butanone) VOL7

0 0.015 13 VOL NO Vinyl Acetate VOL59

0 0.01 25 VOL YES Dibromomethane VOL35

0 0.01 36 VOL YES 1,1,1,2-Tetrachloroethane VOL29

0 0.015 43 VOL YES 1,2,3-Trichloropropane VOL31

0 0.025 90 90 VOL NO Acrylonitrile MAH12

0 0.025 91 91 VOL NO Chloroprene CLPRENE 

## List of Surrogates

Code Surrogate Description MDL Criteria "A"

D4-CL2ETH2 D4-CL2ETH2 D4-1,2-Dichloroethane D4-CL2ETH2

D8-TOL D8-TOL D8-Toluene D8-TOL

BROMOF BROMOF Bromofluorobenzene BROMOF

D10-ETHY2 D10-ETHY2 D10-Ethylbenzene (FS) D10-ETHY2


## List of Spikes

Code

MVOCB

Page 2 of 2H Test Code : VOCCOND-W English Test Name : VOST Condensate (8260Cmod) Description : Determination of volatile aromatic and halogenated organics in liquid by purge and trap GC/MS.

Result Units : ug/L
Reference Number : BRL SOP-00305

List of Parameters

Code Parameter Description RDL
HAL28 Dichlorodifluoromethane (FREON 12) 1
HAL1 Chloromethane 2
HAL2 Vinyl Chloride 0.4
HAL3 Bromomethane 3
HAL4 Chloroethane 1
HAL5 Trichlorofluoromethane (FREON 11) 2
VOL1 Acetone (2-Propanone) 15
HAL6 1,1-Dichloroethylene 0.5
HAL 43 Iodomethane 0.6
VOL3 Carbon Disulfide 0.5
HAL7 Methylene Chloride(Dichloromethane) 1
HAL9 1,1-Dichloroethane 0.4
VOL59 Vinyl Acetate 1.5
HAL8 trans-1,2-Dichloroethylene 1
HAL10 cis-1,2-Dichloroethylene 1
HAL11 Chloroform 0.4
HAL15 1,2-Dichloroethane 0.5
VOL7 Methyl Ethyl Ketone (2-Butanone) 10
HAL12 1,1,1-Trichloroethane 0.5
HAL14 Carbon Tetrachloride 0.5
MAH1 Benzene 0.5
HAL22 1,1,2-Trichloroethane 0.5
HAL17 1,2-Dichloropropane 0.5
HAL16 Trichloroethylene 0.5
VOL35 Dibromomethane 0.5
HAL18 Bromodichloromethane 0.4
HAL20 cis-1,3-Dichloropropene 0.4
HAL21 trans-1,3-Dichloropropene 0.6
HAL24 Dibromochloromethane 0.4
VOL6 Methyl Isobutyl Ketone 10
VOL60 Methyl Butyl Ketone (2-Hexanone) 10
MAH2 Toluene 0.5
VOL62 Ethylene Dibromide 0.5
HAL23 Tetrachloroethylene 0.5
CB1 Chlorobenzene 0.5
VOL29 1,1,1,2-Tetrachloroethane 0.5
MAH3 Ethylbenzene 0.5
MAH13 p+m-Xylene 0.5
MAH7 Styrene 0.5
MAH4 o-Xylene 0.5
HAL26 Bromoform 0.4
HAL27 1,1,2,2-Tetrachloroethane 1
VOL31 1,2,3-Trichloropropane 0.6
CB2 1,3-Dichlorobenzene 0.5
CB3 1,4-Dichlorobenzene 0.5
CB4 1,2-Dichlorobenzene 0.5

List of Surrogates

Code Surrogate Description

D4-CL2ET D4-1,2-Dichloroethane
D8-TOL D8-Toluene
BFB 4-BromofluorobenzeneTest Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 56 of 66 

### Appendix A - EPA ICR Letter – May 15, 2014Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 57 of 66Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 58 of 66Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 59 of 66Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 60 of 66 

### Appendix B - July 14, 2014 EPA Email Regarding PCB Testing1 

### Myers, Jason

To: Thomas Andersen; Fritz, Wesley; Tim Gilder; James Bell; Atsushi Eguchi; Tadayoshi Hiyama; David Blye; David Wise; David Gratson Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

To PVC MACT Working Group:

Per Jodi Howard’s reply below, PCB testing is not required for the 2014 PVC Process Vent Section 114 Request. I have
asked her to clarify that same requirement for the PVC MACT compliance performance test. I will keep you informed on her reply.

Regards,

Rich

Richard Krock

Technical Director

The Vinyl Institute 1737 King Street Suite 390 Alexandria, VA 22314 Direct: 571.970.3392 Mobile: 571.216.4474 Fax: 571.970.3271 Email: rkrock@vinylinfo.org http://www.vinylinfo.org http://www.vinylindesign.com

From: Richard Krock Sent: Monday, July 14, 2014 5:22 PM To: 'Howard, Jodi'; Bouchard, Andrew Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

Dear Ms. Howard,

Thank you for the quick response on the 2014 PVC Process Vent Section 114 Request. Does this same answer apply for those companies seeking to use this S114 test as their compliance performance test for the PVC
MACT? Again, thank you for the clarification.

From: Howard, Jodi [ mailto:Howard.Jodi@epa.gov ] Sent: Monday, July 14, 2014 3:09 PM To: Richard Krock; Bouchard, Andrew2 Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

Mr. Krock,

Testing for polychlorinated biphenyls is not required for the 2014 PVC process vent 114.

Thanks.

From: Richard Krock [ mailto:rkrock@vinylinfo.org ]
Sent: Monday, July 14, 2014 11:46 AM
To: Bouchard, Andrew; Howard, Jodi
Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on PCB Testing in EPA S114 for Process Vents

Dear Mr. Bouchard,

Thank you for the responses to our earlier questions on the S114 for Process Vents. We have an additio nal clarification regarding PCB testing as explained in the attached letter. Your quick response is
needed and will be highly appreciated. Please do not hesitate to contact me with any questions on this

matter.

Thank you.

Richard Krock

Technical Director

The Vinyl Institute 1737 King Street Suite 390 Alexandria, VA 22314 Direct: 571.970.3392 Mobile: 571.216.4474 Fax: 571.970.3271 Email: rkrock@vinylinfo.org http://www.vinylinfo.org http://www.vinylindesign.com

From: Bouchard, Andrew [ mailto:Bouchard.Andrew@epa.gov ] Sent: Friday, July 11, 2014 3:44 PM To: Richard Krock; Howard, Jodi Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Mr. Krock,3 Per the email below, attached you will find a consolidated Q&A document consisting of all the questions VI has raised on EPA’s CAA Section 114 request related to the Excel surveys & instructions, process wastewater and/or resin sampling, and process vent testing. Again, I’d just
like to note that if any facility has site sp e cific issues on how to comply with our CAA section 114 request, they should contact us directly. Thanks.

___________________________________ Andrew Bouchard Environmental Engineer U.S. Environmental Protection Agency OAR/OAQPS/SPPD/RCG Phone: (919) 541-4036 Fax: (919) 541-0246 Bouchard.Andrew@epa.gov

From: Bouchard, Andrew
Sent: Tuesday, July 01, 2014 4:17 PM
To: 'Richard Krock'; Howard, Jodi
Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Mr. Krock,

We are in the process of putting together a consolidated Q&A document consisting of all the questions VI has raised on EPA’s CAA Section 114 request rela ted to the Ex cel surveys & instructions, process wastewater and/or resin sampling, and process vent testing. Portions of
VI’s specific questions related specifically to the process wastewater and/or resin sampling have already been responded to (see email from May 22, these answers will be consolidated into the Q&A document for ease and consisten c y) and EPA is expecting responses from those facilities
asked to provide us with this data by July 31, 2014. We anticipate responding to the remaining
issues raised by VI in the aforementioned consolidated Q&A document by no later than next week. Thanks for your pati ence and hop e you all have a happy fourth of July weekend!

___________________________________ Andrew Bouchard Environmental Engineer U.S. Environmental Protection Agency OAR/OAQPS/SPPD/RCG Phone: (919) 541-4036 Fax: (919) 541-0246 Bouchard.Andrew@epa.gov

From: Richard Krock [ mailto:rkrock@vinylinfo.org ]
Sent: Tuesday, July 01, 2014 2:22 PM
To: Howard, Jodi; Bouchard, Andrew
Cc: Lassiter, Penny; Kataoka, Mark; JC Walker Subject: RE: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Dear Ms. Howard and Mr. Bouchard:

Could you provide a status update on the response requested in the e

‐ mail below? Tha nk you.4 Richard Krock

Technical Director

The Vinyl Institute 1737 King Street Suite 390 Alexandria, VA 22314 Direct: 571.970.3392 Mobile: 571.216.4474 Fax: 571.970.3271 Email: rkrock@vinylinfo.org http://www.vinylinfo.org http://www.vinylindesign.com

From: Richard Krock Sent: Friday, June 13, 2014 4:35 PM To: Howard, Jodi ( Howard.Jodi@epa.gov ); Bouchard, Andrew ( Bouchard.Andrew@epa.gov )
Cc: Penny Lassiter ( lassiter.penny@epa.gov ); Kataoka, Mark ( Kataoka.Mark@epa.gov );
JC Walker Subject: VI PVC MACT Subgroup Questions on EPA S114 for Process Vents

Dear Ms. Howard and Mr. Bouchard:

The Vinyl Institute’s PVC MACT Subgroup on Process Vents has raised questions regarding EPA’s May 15, 2014 Section 114 Request for PVC producer’s Process
Vents. The Subgroup’s questions are contained in the attached letter. The Vinyl
Institute appreciates the Agency’s time to review the questions and look forward to

your response. Please do not hesitate to contac t me with any questions in this regard.

Thank you.

Richard Krock

Technical Director

The Vinyl Institute 1737 King Street Suite 390 Alexandria, VA 22314 Direct: 571.970.3392 Mobile: 571.216.4474 Fax: 571.970.3271 Email: rkrock@vinylinfo.org http://www.vinylinfo.org http://www.vinylindesign.com The linked image cannot be displayed. The file may have been moved, renamed, or deleted. Verify that the link points to the co rrect file and location.Test Plan for EPA ICR – Shintech Louisiana LLC

H:\HOUSTON IAS\PROJECTS WESTON (HOU)\SHINTECH LOUISIANA LLC\PROTOCOL\SHINTECH LOUISIANA LLC ‐ ICR PROTOCOL 07242014.DOCX Page 66 of 66 

### Appendix C - Enclosure 1, Attachment B and C

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 1 05/15 /2014 

### MAXIMUM ACHIEVABLE CONTROL TECHNOLOGY (MACT) STANDARDS DEVELOPMENT INFORMATION COLLECTION REQUEST

I. Introduction

Under the authority of Section 114 of the Clean Air Act, this information collection request is to be completed for operations that comprise the Polyvinyl Chloride and Copolymers (PVC) source category at your company. The PVC Production source category includes any facility which manufactures polymerized vinyl chloride. PVC is be produced by the suspension, suspension blending, emulsion/dispersion or bulk processes, although other methods may be used. The source category includes the collection of all equipment and activities necessary to produce PVC ho mopolymer or copolymer resin.

This information collection request consists of two parts: (1) completion of information collection request response forms (survey) and submission of supplemental data and information; and (2) testing and analysis of emissions from PVC process vents (i.e., at the outlet of the final control device). The results of testing are reported in either the Electronic Reporting Tool (ERT) or in dedicated worksheets that are contained in a single Microsoft Excel workbook file along with the required response forms. Except for the required testing, complete this information collection request as completely as possible from best available existing information from the 2013 calendar year.

Instructions for obtaining the information collection request response forms are in Section II of this enclosure. A summary of the supplemental data and information requested in this information collection request is in Section III. Instructions for submitting your response are in Section IV. Section V contains general instructions for completing your response and includes specific guidance for completing each response form. For your convenience, we have provided additional information on the scope and purpose of this information collection request, as well as useful definitions, in Attachment A. Respondents should read this material before attempting to complete the response forms. Respondents may also wish to review the rule and implementation information for PVC production before completing the response forms by visiting the EPA’s Technology Transfer Network

– Air Toxics Web Site for PVC:

http://www.epa.gov/ttn/atw/pvc/pvcpg.html

Additional information on the PVC process vent testing and analysis requirements can be found in Attachment B of this enclosure. Information regarding how to calculate and report method detection levels in located in Attachment C of this enclosure.

If you have questions regarding this request, please contact Ms. Jodi Howard, Refining and Chemicals Group, at (919) 541-4607 or howard.jodi@epa.gov

.

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 2 05/15 /2014 

### II. Instructions for Obtaining the Information Collection Request Files

The information collection request response forms are available as a single Microsoft Excel 2007 workbook. The workbook is included with this enclosure and is titled:

“ 2014 PVC 114 PV Testing.xlsx ”



### The workbook should be completed for the entire PVC production facility. Before submitting the file, the file name will be changed to reflect the actual company and facility ( see Section III).

Other files included in this package are an example of how to complete the Excel workbook and a copy of this enclosure. Where necessary, examples of how to complete selected portions of the information collection request response forms are included directly in the forms themselves. Refer to examples and the instructions contained in this enclosure when completing

your response.

III. Supplemental Data and Information Requested

We are requesting you submit supplemental data and information to support the information submitted in the information collection request response forms. The following table summarizes the supplemental data and information that must be submitted with your response. Provide actual recorded data where possible and submit that data in Microsoft Excel format. If recorded process data (such as CEMS data) are not available, then provide estimates based on engineering assessments, material balances, etc. and provide copies of estimation worksheets and other supporting documentation. Recorded process data, sampling results, test results, estimation worksheets, engineering calculations, assessments, etc. must be provided to support the information submitted for all parts of the information collection request response.

Except for the results of PVC process vent testing, the information provided in response to this information collection request should be from the best available existing information from the 2013 calendar year.

Supplemental Data and Information Related Equipment, Stream, Emission Point Time Period

Process Unit Plot Plan Process Unit N/A Process Unit Flow Diagram Process Unit N/A HAP/Total VOC Concentration, Emissions Data or Estimates All Uncontrolled Emission Points 2013

Safety/Pressure Relief Notifications and estimates of emissions from releases Process Unit Safety/Pressure Relief Devices 2013

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 3 05/15 /2014 

### IV

. Instructions for Submitting Your Information Collection Request Response

Use the appropriate file naming format as listed below for the files you submit when responding to this information collection request:

Submission File Name Format

Completed Response Workbook 2014 PVC 114 PV Testing.xlsx

Plot Plan [Company]_[Facility] _PlotPlan

Process Flow Diagram [Company]_[Facility] _PFD

Data/Estimates [Company]_[Facility]_[ProcessUnitID]_[ProcessVent/EmissionPoint/Stream/Waste waterStream/ProcessEquipment/ControlEquipment ID]_[YYYYMMDD]to[YYYYMMDD]



### For file names that include dates or date ranges, use four digits for the year (YYYY), two digits for the month (MM), and two digits for the day (DD).

EXAMPLE

Generic Chemical Corporation has a manufacturing facility in Anytown, USA

According to the instructions in Section II and IV, the files would be renamed as:

Submission File Name

Completed Response Workbook PVC ICR _Generic_Anytown.xls



### and submitted with all other required data and information outlined Section III.

All recipients must perform the requested stack testing and submit the test results, reports, and documentation along with the responses to the information collection request and supplemental data and information specified in Attachments A, B and C of Enclosure 1 no later than November 17 , 2014 . Any submissions made after this date will be in violation of this Section 114 request.

Please e-mail the completed non-confidential response to:

CCG -PVC@epa.gov

If you are submitting confidential business information (CBI) as described in Enclosure 2, then this information must be mailed to EPA in hard-copy or on a CD-ROM or
DVD -ROM disk. Clearly mark the disk and/or the materials with the words “Confidential

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 4 05/15 /2014 

### Business Information” and send either via U.S. Postal Service Express Mail, registered mail, or private courier to: Jodi Howard

U.S. EPA Office of Air Quality Planning and Standards Sector Policies and Program Division, Refining and Chemicals Group Mail Code E143-01 Research Triangle Park, NC 27711

Additionally, if you are submitting CBI via mail in hard-copy or on CD-ROM or DVDROM disk, you must also submit a non -CBI version of your information collection request response to the email address listed above. DO NOT ELECTRONICALLY TRANSMIT CONFIDENTIAL BUSINESS INFORMATION TO EPA.

If you have questions regarding this request, please contact Ms. Jodi Howard, Re fining and Chemicals Group, at (919) 541-4607 or howard.jodi@epa.gov.

V. Background Information and Instructions for Completing the Information Collection Request Response Forms

NOTE: For the purposes of this information collection request, all HAP and VOC

concentrations and emissions are to be quantified. Do not report concentrations or emissions as “trace” or “minimal.” If a concentration is at or below a detection limit, then provide the detection limit.

Form A

– Company Information and Facility Information

 

### Forms A-1 and A-2 are where the respondent company and facilities are identified.

 

### In question I.1 of Form A-1, identify the legal parent company/legal corporate owner name. In questions I.2 through I.6 provide the mailing address for the legal parent company/legal corporate owner.

 

### Identify the size of the company by selecting the appropriate range for the number of employees (including all subsidiaries, branches, and related establishments owned) in question I.7.

 

### On Form A-2, provide the facility name and address information requested in question II.1, including the latitudinal and longitudinal coordinates of the facility. Facility latitudes and longitudes should be reported in decimal degrees to the 5 th 

### decimal place, and longitudes should include negative sign, e.g. (37.91986, -87.32724 ) Sources of these data include EPA permits (e.g., NPDES permits), county property records, facility blueprints, and site plans.

 

### Provide the name and contact information for the facility’s technical contact in q uestions III.1 through III.3 on Form A-2.

 

### On Form A-2

, Section IV, respondents are asked to identify whether the facility is a major source of HAP emissions by selecting “Yes,” or “No,” in question IV.1. Section 112(a)(1) of the CAA defines a major source as any stationary source or group of stationary sources located within a contiguous area and under common control that emits or has the potential to

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 5 05/15 /2014 

### emit considering controls, in the aggregate, 10 tons per year or more of any hazardous air pollutant or 25 to ns per year or more of any combination of hazardous air pollutants. Affected sources that have not yet commenced production of PVC resin or that are expanding existing production capacity are asked to complete all parts of this information collection request. For those sources, projected actual emissions (not “Potential to Emit”) are requested in lieu of actual operating emissions.

 

### For facilities that are not major sources of HAP emissions (and select “No” for question IV.1), the respondent is asked to identify if and when a permit limit for their potential HAP emissions to avoid being classified as a major source in questions IV.2 and IV.3, respectively was taken.

 

### Indicate if the facility manufactures other products in addition to PVC resin by selecting “Yes,” or “No,” for question IV.4 on Form A

- 2. If “Yes,” list the other products manufactured in the response field for question IV.5.

 

### Indicate if there are any HAP emission associated with any co-located facilities by selecting “Yes,” or “No,” for questio n IV.6 on Form A-2.

Form B

– Control Devices, Recovery Systems, and Process Equipment

 

### Prior to completing the remainder of the forms (i.e., forms B through N), you should complete a plot plan (plant layout schematic) and process flow diagram(s) for the PVC production facility. Do not submit “block flow diagrams.” The level of detail requested is more than generally contained in “block flow” diagrams but less than that generally contained in piping and instrumentation diagrams (P&IDs). Process flow diagrams should accurately show ALL:

o Process equipment;

o Recovery systems including all recovery equipment;

o Process wastewater treatment systems including all wastewater treatment equipment;

o Closed vent systems ( identify the collection of piping for each closed vent system using a dotted-line boundary on the process flow diagram );

o Control devices ( also clearly show any piping configurations that allow a gaseous stream routed to a closed vent system and control device to bypass the control device );

o Pressure relief devices (PRDs); and

o Emission points;

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 6 05/15 /2014  

### Each item in the table below is to be given a unique identifier in the form of Z- x, where “Z” is a unique code for each item listed in the table below and x = 1, 2, 3,...n. The unique identifier should exactly match between the process flow diagram and information provided in the completed response workbook(s). Refer to Attachment A of this Enclosure for relevant definitions.

Control devices (C

- x) Recovery systems (RS

- x) Individual recovery equipment that comprise the recovery system (RE

- x) Individual wastewater treatment equipment that comprise each process wastewater treatment system (WWE

- x)

Process equipment (U

- x) Emission points (EP

- x) Pressure relief devices (PRD

- x) Closed vent systems (CVS

- x)

Form B-1

– Control Devices

General Instructions

 

### Each control device should be listed in Form B-1.

 

### For the purposes of this information collection request, wastewater collection, handling and treatment equipment (including process wastewater steam strippers) are considered wastewater treatment equipment and not control or recovery devices.

 

### For each control device, submit a copy of the most recent emissions test report. The report should include information on the process operations that influenced emissions during the test, including the resin type being produced. Include information such as the purpose of the test, when it was conducted and what test methods were used. If emissions test reports are not available, calculations based on emission factors, material balances, or engineering principles must be submitted and supported by submitting a step- by -step description of the calculations, including assumptions used and a brief rationale for the validity of the calculation method used. (See guidance documents listed in Attachment A, Section IV).

 

### For the following control devices, complete the appropriate Forms: absorbers - Form F-1; thermal or catalytic oxidizers - Form F-2 ; and, condensers - Form F-3.

Specific Instructions by Form Column

 

### Column 1: Each control device is to be given a unique code or identifier in the form of C-x, where x = 1, 2, 3,...n, in Form B -1. This unique code/identifier should exactly match the identifier used in the process flow diagram and will be used on subsequent forms.

### Enclosure 1

PVC Section 114 Enclosure 1

– Page 7 05/15 /2014  

### Column 2: Select the type of control device from the list provided in the Form.

 

### Column 3 : If “other” was selected in column 2, provide a description of the control device.

 

### Column 4: Each emission point from a control device (or from the last control device in a series) that exhausts directly to the atmosphere should be shown on the process flow diagram and is to be given a unique code or identifier of the form EP- x, where x = 1,2,3,...n in Form B-1. This unique code/identifier will be used on subsequent forms. If the exhaust stream from the control device immediately enters a subsequent control device (e.g., exhaust from a thermal oxidizer is routed to an acid gas scrubber) provide the subsequent control device identifier instead of the emission point identifier.

Form B-2

– Recovery Systems and Closed Vent Systems

General Instructions

 

### Each recovery system should be listed in Form B-2.

 

### For the purposes of this information collection request, wastewater collection, handling and treatment equipment (including process wastewater steam strippers), are considered wastewater treatment equipment and not control or recovery systems.

 

### If you use a condenser as part of a recovery system, and emissions from the condenser are routed directly to the atmosphere without first passing through a control device, complete Form F-3 for the condenser(s).

Specific Instructions by Form Column

Table 1

 

### Column 1: Each recovery system is to be given a unique code or identifier in the form of RSx, where x = 1, 2, 3,...n, in Form B -2. This unique code/identifier should exactly match the identifier used in the process flow diagram and will be used on subsequent forms.

 

### Column 2: Provide a description of the recovery system.

 

### Column 3: Indicate if, at any point in the recovery or closed vent system, emissions can be discharged directly to the atmosphere. If you answer yes, complete Table 2.

 

### Columns 4-6 : List the control devices that control emissions from the recovery and closed vent system. The control device ID(s) that you provided on Form B-1 will be available as a pick list in columns 4 through 6.

Table 2

 If you answered “Yes” in column 3 of Table 1, complete Table 2.

 Column 1: Identify the recovery system ID. The recovery system ID(s) that you provided in Table 1 will be available as a pick list in column 1 of Table 2.

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###  Column 2: Identify each emission point that discharges directly to the atmosphere. Do not list emission points for streams exiting the recovery system that are routed through a closed vent system to a control device. Each emission point that exhausts directly to the atmosphere should be shown on the process flow diagram and given a unique code or identifier of the form EP- x, where x = 1,2,3,...n in Form B -2. This unique code/identifier will be used on subsequent forms.

 Column 3: Identify if the emission point is used as a bypass for the control device, or, if the emission point is a process vent.

 Column 4: Indicate if the equipment opening standards in 40 CFR Part 61, subpart F are met before a discharge occurs through the emission point.

Table 3

 

### Column 1: Each piece of recovery equipment included in the recovery system should be shown on the process flow diagram and given a unique code or identifier of the form RE-x, where x = 1, 2, 3,...n, in Table 2 of Form B -2. This unique code/identifier will be used on subsequent forms.

 

### Column 2: Provide a description of the recovery equipment.

 

### Co lumn 3: Indicate recovery system ID to which the recovery equipment belongs. The recovery system ID(s) you provided in Table 1 will be available as a pick list in column 3.

Form B-4

–

Process Equipment

General Instructions

 

### All remaining process equipment should be listed on Form B-4. Do not list any equipment previously noted on Forms B-1 through B-2

.

 

### Process equipment may be grouped on the process flow diagram if and only if the individual pieces of equipment in the group are of identical design and all process vents exiting each piece of process equipment are routed to the same control device.

 

### If emissions from a condenser (not previously listed as part of a recovery system) are routed directly to the atmosphere without first passing through a recovery system or control device, complete Form F-3 for the condenser(s).

Specific Instructions by Form Column

 

### Column 1: Each piece of process equipment is to be given a unique code or identifier in the form of U- x, where x = 1, 2, 3,...n, in Form B -4. This unique code/identifier should exactly match the identifier used in the process flow diagram and will be used on subsequent forms.

 

### Column 2: Provide a description of the process equipment.

 

### Column 3: Provide an indication if emissions from the process equipment are routed directly to the atmosphere without passing first through a recovery system or control device.

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### Column 4-6: If you answered “Yes” in column 3, list the emission point ID(s). Each emission point should be shown on the process flow diagram and is to be given a unique code or identifier of the form EP- x, where x = 1,2,3,...n in Form B -4. This unique code/identifier will be used on subsequent forms. If the emission point is controlled (and therefore listed in Form B-1) do not duplicate the emission point in Form B-4; only list uncontrolled emission points.

 

### Column 7: If you answered “No” in column 3, indicate if emissions from the process equipment are routed to a recovery system.

 

### Column 8: If you answered “Yes” in column 7, select the appropriate recovery system ID entered on Form B-2.

 

### Column 9-11: If you answered “No” in column 7, list the control device identifiers previously identified on Form B-1. If emissions are controlled by multiple control devices, list each control device identifier in the order of control (e.g., the overhead stream from aresin stripper (U-1) is controlled by 1) a thermal oxidizer (C-1) and an acid gas scrubber (C2)).

Form F

– Control Devices

General Instruction

 

### Complete Form F-1 for each absorber used as a control device, or for any absorber that emits directly to the atmosphere.

 

### Complete Form F-2 for each thermal or catalytic oxidizer.

 

### Complete Form F-3 for each condenser used as a control device or for any condenser that emits directly to the atmosphere.

Specific Instructions by Form Row

Form F-1

 

### Rows 1-2: Select the type of equipment (i.e., control device, recovery equipment or process equipment). Then in row 2, select the equipment ID you entered into the corresponding Form
B.

 

### Rows 3-4 : Select the type of absor ber from the pick list. If “other,” provide a description of the absorber type in row 4.

 

### Rows 5-14 : Provide the operating characteristics of the absorber in rows 5 through 14. Provide as much of the information as possible.

 

### Rows 15-16: Indicate the year the equipment was installed and cite any applicable regulations.

Form F-2

 

### Row 1: Select the control device ID (based on the values you entered in Form B-1).

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### Rows 2-3 : Provide the number of operating hours per year and indicate if the device is considered emergency equipment.

 

### Row 5: Indicate the type of oxidizer (i.e., thermal or catalytic).

 

### Rows 6 -35: Provide the design parameters and operating characteristics requested in rows 6 through 35. Complete as much of the information as possible for each oxidizer.

 

### Rows 36-37: Indicate the year the equipment was installed and cite any applicable regulations.

Form F-3

 

### Rows 1-2: Select the type of equipment (i.e., control device, recovery equipment, or process equipment). Then in row 2, select the equipment ID you entered into the corresponding Form
B.

 

### Rows 3-4 : Select the type of condenser from the pick list. If “other,” provide a description of the condenser type in row 4.

 

### Rows 5-12 : Provide the operating characteristics of the condenser in rows 5 through 12. Provide as much of the information as possible.

 

### Rows 15-16: Indicate the year the equipment was installed, and cite any applicable regulations.

Form H

– Equipment Leaks

 

### Complete Form H for equipment leaks at the PVC production facility.

 

### Provide information regarding your facility’s leak detection and repair (LDAR) program in Table 1.

 

### In Table 2, provide equipment counts for all equipment at your facility in the source category. In addition, provide the subtotal of the equipment that are associated with your closed vent system(s).

 

### In addition to completing Form H, submit a copy of the leak detection and repair procedures for the facility.

Form I

– Equipment Opening

Table 1

 

### Complete this Form for each piece of process equipment, recovery equipment and any additional equipment that is not assigned an equipment ID (e.g., in-line filters).

 

### Complete a separate Form I for each piece of process equipment, recovery equipment or other equipment that was opened in 2013. Identify the equipment (by selecting the recovery or process equipment ID from Forms B-2 or B-4 if applicable). Indicate the number of times the equipment was opened during 2013 and the reasons for opening the equipment (list all that apply). Provide the equipment volume in cubic meters.

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### Indicate how the HAP concentration of the equipment is determined, and how (if at all) HAP emissions are controlled.

Table 2

 

### In Table 2, list the individual HAP present in the equipment and the concentration of each HAP at the equipment opening.

 

### Provide the total mass of each HAP emitted from opening the equipment in 2013, and a basis for the emissions values. Values should be reported for normal operations; not for startups, shutdowns, or malfunctions.

 

### Provide copies of estimation worksheets and any other relevant documentation.

Form K-1

– Tanks, Vessels, and Portable Containers Used for Feedstock Storage, Product Storage, Vent Gas Storage, Holding, and Wastewater

 

### Complete a separate Form K-1 for each tank, vessel portable container used for feedstock storage, product storage, holding and wastewater, including surge control vessels that are used to hold process vent gas prior to the control device for 2013 only. Do not include gas holders on Form K-1 (refer to Attachment A, Section V of this Enclosure for the definition of a gas holder).

 

### In Table 1, identify the process equipment by selecting the equipment ID provided on Form B-2 or Form B-4 (if applicable). If the equipment was not identified on Form B-2 or B-4, provide an equipment description.

 

### Provide a detailed description of the equipment, and include (if applicable) if the tank is a fixed, floating internal, or floating external roof.

 

### Select the purpose of the equipment from the pick list provided. If none of the options on the pick list accurately describe the purpose of the equipment, please select “Other” and specify the purpose in the next row.

 

### Indicate the number of turnovers for 2013, the equipment volume and the average storage temperature.

 

### Indicate how the HAP concentration of emissions from the tank/vessel/container are determined and if HAP emissions are controlled, identify the method of control.

 

### In Table 2, indicate the individual HAP contained in the tank/vessel/portable container and the corresponding vapor pressure. Provide concentration values and total emissions for 2013.

 

### Provide copies of estimation worksheets and any other relevant documentation.

Form L

– Startup, Shutdown and Malfunction

 

### Complete Form L for startups, shutdowns and malfunctions during 2013 as completely as possible.

 

### Each column in Form L represents a single startup, shutdown or malfunction event. Provide emissions in total pounds for the event.

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### Submit with your response to this information collection request, copies of all records of emissions during periods of process startup, shutdown and malfunctions for 2013.

Form P

– Process Vent Emissions Testing Data

 

### Form P is used to collect results of performance tests that are not supported by the EPA’s Electronic Reporting Tool (ERT). Refer to Attachment B to this Enclosure 1, Summary of Test Procedures, Methods, and Reporting Requirements for Polyvinyl Chloride and Copolymers Facility Emission Points for more information for additional information.

 

### Copy Form P as necessary for pollutants/compounds sampled on different dates.

 

### For multiple control devices, users may copy Form P within the response workbook.

 

### For each test run, provide the required operating parameters collected during the test. Note the selection for “PVC Production Rate Units.” If your final product is sold and shipped dried (e.g., a suspension resin), select “dry lbs PVC/day.” If your final product is sold and shipped withou t being dried (e.g., an emulsion resin), select “total lbs PVC/day.”

 

### Provide a numerical result for each compound. Do not provide non-numerical data in the compound results columns.

 

### In the “ Run # Detection” columns, identify the status of the measured values relative to detection levels following the instructions in Attachment C to this Enclosure 1, “Guidance for Calculating and Reporting Values Measured Below Method Detection Levels.”

Form Q

– Total Hydrocarbon 30-Day Monitoring

 

### Form Q is used to collect the results of the 30 -day, continuous total hydrocarbon (THC) and methane (CH 4 

### ) monitoring required in Section 1.3 of Attachment B to this Enclosure 1, Summary of Test Procedures, Methods, and Reporting Requirements for Polyvinyl Chloride and Copolymers Facility Emission Points.

 

### For multiple control devices, users may copy Form Q within the response workbook.

 

### Along with the continuous 30-day THC and CH 4 

### readings, provide the corresponding oxygen and moisture values, along with the PVC type and grade being manufactured.

 

### Supply the control device temperature, and the control device and THC monitoring operations indicator.

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## Background for Polyvinyl Chloride and Copolymers Production MACT Standards Development Information Collection Request

1.0 Introduction

The purpose of this attachment is to provide the respondent with additional detail on the relevant requirements of the Clean Air Act, the regulatory background of the polyvinyl chloride and copolymers production source category, and to provide a list of definitions of key terms used in the information collection request.

2.0 Summary of Clean Air Act Requirements

The maximum achievable control technology (MACT) standards development information collection request was developed by the U. S. Environmental Pro tection Agency’ s (EPA) Office of Air Quality Planning and Standards Emission Standards Division (OAQPS/ESD) to help EPA meet its obligations under the Clean Air Act Amendments of 1990. Specifically, the Clean Air Act Amendments require EPA to develop regulations under Section 112(d) to limit emissions of hazardous air pollutants (HAP) from major and area sources of emissions. Section 11 2(a)(1) defines a major source as “ any stationary source or group of stationary sources located within a contiguous area and under common control that emits or has the potential to emit considering controls, 10 tons per year or more of any hazardous air pollutant or 25 tons per year or more of any combinati on of hazardous air pollutants.” Based on the Administrator’ s determination, EPA may lower the major source cutoff for individual HAP. An area source is “ any stationary source of hazardous air pollutant s that is not a major source.”

The Clean Air Act Amendments of 1990 prescribe an analytical framework that EPA is to apply in developing national emission standards for hazardous air pollutants (NESHAP) for major sources. A key concept in this framework is the establishment of the MACT floor. The amendments specify that NESHAP for existing sources in a particular category or subcategory are to be no less stringent (but may be more stringent) than the average emission limitation achieved by the best performing 12 percent of the existing sources in such category or subcategory of sources. In categories or subcategories with less than 30 sources, the floor is to be based on the average emission limitation achieved by the best performing 5 sources. The MACT floor for new sources is the emission control that is achieved in practice by the best controlled similar source.

The Clean Air Act Amendments allow the EPA Administrator to "distinguish among classes, types, and sizes of sources within a category or subcategory in establishing such standards" (Section 112(d)).

3.0 Regulatory Background for the Polyvinyl Chloride and Copolymers Production Source Category

On October 21, 1976, EPA promulgated emission standards for vinyl chloride under the risk -based standard then in effect (41 FR 46560; 40 C.F.R. Subpart F (§§ 61.60 - 61.71); “the Part 61 NESHAP”)

. When Congress amended the CAA in 1990, it required EPA to implement

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### te chnology based standards. As a result, EPA proposed MACT standards for the Polyvinyl Chloride and Copolymers Production source category on December 8, 2000 (65 FR 76958) and promulgated final MACT standards for the source category on July 10, 2002 (67 FR 45886) (“the Part 63 NESHAP”)

. EPA adopted most of the Part 61 NESHAP as the new Part 63 NESHAP and the Part 61 standards became the MACT floor for existing sources.

Mossville Environmental Action NOW and Sierra Club petitioned the U.S. Court of Appeals of the District of Columbia to review various provisions of the Part 63 NESHAP. The Part 63 NESHAP was vacated on June 18, 2004 in Mossville v. EPA, 370 F. 3d. 1232 (D.C.Cir. 2004) and remanded to the agency for it to reconsider or properly explain its methodology for regulating HAPs emitted in PVC production other than vinyl chloride by use of a surrogate.

On April 17, 2012, the EPA promulgated revised standards for PVC major and area sources. After promulgation, the Administrator received petitions for reconsideration of certain provisions in the final rules.

The purpose of the current information collection is to gather data from PVC production facilities that were either not included in the EPA’s previous data collection efforts for the source category or whose data were excluded by the Agency from various technical analyses that supported the April 2012 rulemaking. The collected data will support analyses of environmental and economic impacts of various revisions to the current Part 63 NESHAP for PVC major and

area sources.

4.0 Guidance Documents

Following is a list of EPA guidance documents and resources that may be useful to respondents in estimating HAP emissions.

1. Compilation of Air Pollutant Emission Factors: Volume I: Stationary Point and Area Sources. U. S. Environmental Protection Agency. Research Triangle Park, N.C. 1995. http://www.epa.gov/ttn/chief/ap42/index.html

2. Factor Information Retrieval (FIRE) Data System. U. S. Environmental Protection Agency. http://cfpub.epa.gov/oarweb/index.cfm?action=fire.main

3. Protocol for Equipment Leak Emission Estimates. U. S. Environmental ProtectionAgency. Research Triangle Park, N.C. November 1995. Publication No.: EPA45 3 /R-9 5-01 7

.

4. Batch Process ACT. U. S. Environmental Protection Agency. Re search Triangle Park, N.C. February 1994. Publication No.: EPA-453/R-94 -020.

5.0 Key Term Definitions

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### The following definitions are provided for the purpose of the information collection request only. They are not intended to replace statutory definitions or regulatory definitions developed elsewhere.

Bulk process/ resin : A process for producing polyvinyl chloride resin that is characterized by a two

- step anhydrous polymerization process: the formation of small resin particles in a pre

polymerized reactor using small amounts of vinyl chloride monomer, an initiator, and agitation; and the growth of the resin particles in a post polymerization reactor using additional vinyl chloride monomer

. Resins produc ed using the bulk process are referred to as bulk resins.

Control device : A combustion device, recovery device, recapture device, or any combination of these devices used to comply with a regulation, numerical emission limit, work practice standard, etc. Process condensers are not control devices.

Dispersion process/resin : A process for producing polyvinyl chloride resin that is characterized by the formation of the polymers in soap micelles that contain small amounts of vinyl chloride

monomer

. Emulsifie rs are used to disperse vinyl chloride monomer in the water phase. Initiators used in the dispersion process are soluble in water. Resins produced using the dispersion process are referred to as latex or dispersion resins.

Feedstock: Raw ma terial/input to the process unit

.

Gas Holder: A surge control vessel with a bell that is floating in a vessel filled with water that is used to store gases from the PVC production process prior to being recovered or sent to a process vent control device. The bell rises and falls as low

pressure gases enter and leave the space beneath the bell and the water provides a seal between the enclosed gas within the floating bell and the ambient air.

Hazardous Air Pollutants (HAP): See 42 U.S.C. §7412(a)(6).

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### Maintenance wastewater: Wastewater generated by the draining of process fluid from components in the PVCPU into an individual drain system prior to or during maintenance activities. Maintenance wastewater can be generated during planned and unplanned shutdowns and dur ing periods not associated with a shutdown. Examples of activities that can generate maintenance wastewaters include descaling of heat exchanger tubing bundles, hydroblasting PVCPU process components such as polymerization reactors, vessels and heat exchan gers, draining of low legs and high point bleeds, draining of pumps into an individual drain system, draining of portions of the PVCPU for repair and water used to wash out process components or equipment after the process components or equipment has alrea dy been opened to the atmosphere.

Malfunction: A ny sudden, infrequent, and not reasonably preventable failure of air pollution control and monitoring equipment, process equipment, or a process to operate in a normal or usual manner which causes, or has th e potential to cause, the emission limitations in an applicable standard to be exceeded

. Failures that are caused in part by poor maintenance or careless operation are not malfunctions. (40 CFR 63.2)

Polyvinyl Chloride and Copolymers Production Facility: The collection of all polyvinyl chloride and copolymers production process unit, storage vessels, surge control vessels, heat exchange systems, wastewater, and process wastewater treatment systems that are associated with producing polyvinyl chloride.

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### Pol yvinyl Chloride and Copolymers Production Process Unit or PVCPU: A collection of process components assembled and connected by hard

- piping or duct work, used to process raw materials and to manufacture polyvinyl chloride and/or polyvinyl chloride copolymer s. A PVCPU includes, but is not limited to, polymerization reactors; resin stripping operations; resin blend tanks; resin centrifuges; resin dryers; resin product separators; recovery devices; reactant and raw material charge vessels and tanks; holding tan ks, mixing and weighing tanks; finished resin product storage tanks or storage silos; finished resin product loading operation; connected ducts and piping; equipment including pumps, compressors, agitators, pressure relief devices, sampling connection syst ems, open

- ended valves or lines, valves and connectors and instrumentation systems. A PVCPU does not include chemical manufacturing process units, as defined in §63.101, that produce vinyl chloride monomer or other raw materials used in the PVC polymerizat ion

process.

Polyvinyl Chloride and Copolymer Resin (PVC Resin):

Polyvinyl Chloride Copolymer:

Polyvinyl Chloride Homopolymer: The general reference to any PVC homopolymer or copolymer resin manufactured by the suspension, dispersion, bulk , and/or solution processes.

A synthetic thermoplastic polymer that is derived from the simultaneous polymerization of vinyl chloride and another monomer such as vinyl acetate. Polyvinyl chloride copolymer is produced by different processes, including, but

not limited to, suspension, dispersion/emulsion, suspension blending, and solution processes.

Polyvinyl chloride homopolymer means a synthetic thermoplastic polymer that is derived from the polymerization of vinyl chloride and has the general chemical structu re (

- H2CCHCl

- )n. Polyvinyl chloride homopolymer is typically a white powder or colorless granule. Polyvinyl chloride homopolymer is produced by different processes, including (but not limited to), suspension, dispersion/emulsion, blending and bulk

processe s.

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### Process equipment: Any unit operation or group of unit operations or any part of a process or group of parts of a process that are assembled to perform a specific function. Examples of process equipment include, but are not limited to, polymerization
reactors, PVC resin strippers, resin dewatering and dry ing equipment storage tanks and vessels, cooling towers and heat exchange systems, and transfer operations

.

Process unit : The process components assembled and connected by pipes or ducts to process raw and/or intermediate materials and to manufacture an intended product. For the purposes of this information collection request, process unit includes, but is not limited to, polyvinyl chloride production process.

Process wastewater: Wastewater that com es into direct contact with HAP or results from the production or use of any raw material, intermediate product, finished product, by

- product or waste product containing HAP, but that has not been discharged untreated as wastewater. Examples are product ta nk drawdown or feed tank drawdown; water formed during a chemical reaction or used as a reactant; water used to wash impurities from organic products or reactants; water used to cool or quench organic vapor streams through direct contact; water discarded f rom a control device; and condensed steam from jet ejector systems pulling vacuum on vessels containing organics. Gasholder seal water is not process wastewater until it is removed from the gasholder.

Process wastewater stream: Each individual waste strea m exiting an individual piece of process equipment (including, but not limited to, resin stripping equipment, knockout pots, condensers, centrifuges, and scrubbers) prior to being combined with any other stream. Process wastewater streams also include comb ined streams exiting wastewater collection tanks, wastewater treatment equipment/processes, etc.

PVC process wastewater treatment equipment: An individual piece of equipment capable of and normally used for the purpose of removing organic compounds from

a process wastewater stream, used alone or in combination with other PVC process wastewater treatment equipment. Examples include, but are not limited to, wastewater collection, holding, and equalization tanks, wastewater steam and vacuum strippers, and was tewater stripper feed/bottoms heat exchanger.

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### PVC process wastewater treatment system: A collection of PVC process wastewater treatment equipment that removes organic compounds from a process wastewater stream before the process wastewater stream is disch arged from the PVC production facility.

Recovery equipment: Recovery equipment means an individual piece of equipment capable of and normally used for the purpose of recovering chemicals for fuel value (i.e., net positive heating value), use, reuse, sale, and/or destruction or disposal. Examples of equipment that may be recovery equipment include gas holders, compressors, condensers, and liquid separators used to recover vinyl chloride or other feedstocks from gaseous streams such as resin stripper and

was tewater stripper overheads and return those feedstocks for reuse in the resin production process and/or eventual destruction or disposal. For the purposes of this information collection request, wastewater steam and vacuum strippers are considered PVC proc ess wastewater treatment equipment and not recovery equipment.

Recovery system: A recovery system is a collection of recovery equipment. A recovery system typically vents to a control device such as a thermal oxidizer and acid gas scrubber.

Resin grade: T he subdivision of PVC resin that describes it as a unique resin, i.e., the most exact description of a type of resin with no further subdivision . Examples include low molecular weight suspension resins and general purpose suspension resins.

Resin strippe r: A unit that removes organic compounds from a raw polyvinyl chloride and copolymer product. In the production of a polymer, stripping is a discrete step that occurs after the polymerization reaction and before drying or other finishing operations. Exampl es of types of stripping include steam stripping, vacuum stripping, or other methods of devolatilization. For the purposes of this information collection request, devolatilization that occurs in dryers or other finishing operations is not resin stripping. Resin stripping may occur in a polymerization reactor or is a batch or continuous stripper separate from the polymerization

reactor.

Shutdown: T he cessation of operation of an affected source or portion of an affected source for any purpose. (40 CFR 63.2)

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### Startup: T he setting in operation of an affected source or portion of an affected source for any purpose. (40 CFR 63.2)

Stream: Any contained or non

- contained solid, liquid, gas, or vapor entering or exiting an individual unit operation or single piece of equipment.

Stripped resin: The material exiting the resin stripper than contains polymerized vinyl chloride.

Suspension blending process/resin: A process for producing polyvinyl chloride resin that is similar to the suspension polymerization process, but employs a rate of agitation that is significantly higher than the highest range for non

- blending suspension resins. The suspension blending process uses a recipe that creates extremely small resin particles, generally equal to or less than 100 microns in size, with a glassy surface and very little porosity. The suspension blending process concentrates the resins using a centrifuge that is specifically designed to handle these small particles. Polyvinyl chloride resins produced using the suspension blend ing process are referred to as suspension blending resins and are typically blended with dispersion resins.

Suspension process/resin: A process for producing polyvinyl chloride resin that is characterized by the formation of the polymers in droplets of li quid vinyl chloride monomer or other co

- monomers suspended in water. The droplets are formed by agitation and the use of protective colloids or suspending agents. Initiators used in the suspension process are soluble in vinyl chloride monomer. Polyvinyl ch loride resins produced using the suspension process are referred to as suspension resins.

Type of Resin: T he broad classification of PVC homopolymer and copolymer resin referring to the basic manufacturing process for producing that resin, including, but not limited to, suspension, dispersion, bulk , and solution processes.

Volatile Organic Compounds (VOC): See 40 CFR 51.100(s).

Waste management: Handling, treatment, storage, and disposal of waste products.

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### Wastewater: Process wastewater and maintenance wastewater. The following are not considered wastewater for the purposes of this subpart:

(1) Stormwater from segregated sewers; (2) Water from fire

- fighting and deluge systems, including testing of such systems; (3) Spills; (4) Water from safety showers; (5) Samples of a size not greater than reasonably necessary for the method of analysis that is use; (6) Equipment leaks; (7) Wastewater drips from procedures such as disconnecting hoses after cleaning lines; and (8) Noncontact cooling water.

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### 6.0 Key Acronyms and Units of Measure

% percent

a cfm actual cubic feet per minute

acfm/ft 2 

### actual cubic feet per minute per square foot

batches/yr batches per year

B tu /scf British thermal units per standard cubic foot

CAA Clean Air Act

day/yr days per year

DC District of Columbia

d scfm dry standard cubic feet per minute

EPA U.S. Environmental Protection Agency

f t feet

ft/s feet per second

ft 3 

### /1,000 afcm cubic feet per thousand actual cubic feet per minute

g pm U.S. gallons per minute

gr/dscf grains per dry standard cubic foot

HAP Hazardous Air Pollutants

hr/day hours per day

i n inches

in H 2 

### O inches of water

kPa kilopascals

LAER lowest achievable emission rate

lb/day pounds (mass) per day

lb/gal pounds (mass) per U.S. gallon

### Enclosure 1 Attachment A

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### LDAR leak detection and repair

MACT maximum achievable control technology

mg/l milligrams per liter

MMlb/yr million pounds (mass) per year

NAICS North American Industry Classification System

NESHAP National Emission Standards for Hazardous Air Pollutants

OAQPS Office of Air Quality Planning and Standards

oC degrees Celsius

oF degrees Fahrenheit

ohm

- cm ohm

- centimeter

P&ID piping and instrumentation diagram

PFD process flow diagram

ppmv parts per million, by volume

ppmw parts per million, by weight

PVC polyvinyl chloride

S second or seconds

scfm standard cubic feet per minute

SPPD Sector Policies and Programs Division

ton/yr tons per year, or short tons per year

VOC Volatile Organic Compounds

vol% volume percent, or percent by volume

wt% weight percent, or percent by weight

### Enclosure 1 Attachment B

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## Summary of Test Procedures, Methods, and Reporting Requirements for Polyvinyl Chloride and Copolymers Facility Emission Points

This document provides an overview of approved sampling and analysis methods, target reported units of measure, and reporting requirements for polyvinyl chloride and copolymer (PVC) production facilities required to conduct emissions testing and provide emission test data according to the section 114 letter. The purpose for this testing is to gather data on hazardous air pollutant emissions from process vents within this source category. These data will be used to supplement the existing HAP data set for process vents. The document is organized as follows:

1.0 Stack Testing Procedures and Methods

2 .0 How to Report Data

3 .0 How to Submit Data

4 .0 Contact Information for Questions on Test Plan and Reporting

1.0 Stack Testing Procedures and Methods

This information collection request includes stack (performance) test data requests for several pollutants. If you operate a PVC production facility, then you are required to conduct testing as outlined in this document to determine your emissions.

1.1 How to Select Sample Location and Gas Composition Analysis Methods

You must use U.S. EPA Method 1 of Appendix A of p art 60 to select the locations and number of traverse points for sampling. See http://www.epa.gov/ttn/emc/methods/method1.html for a copy of the method and guidance information.

You must use U.S. EPA Method 3A or 3B of Appendix A of part 60 for analysis of flue gas composition, including oxygen concentration. See http://www.epa.gov/ttn/emc/methods/method3a.html for Method 3A or http://www.epa.gov/ttn/emc/methods/method3b.html for Method 3B information.

1.2 Polyvinyl Chloride and Copolymers Production Test Methods and Reporting

Testing must be conducted at the outlet or in the stack of the final control device including, but not limited to, a thermal oxidizer and acid gas scrubber (in series) used to control emissions from PVC production. Table 1.1 summarizes the required test methods for each pollutant, possible alternative methods, and the target reported units of measure.

For copies of the recommended U.S. EPA methods and additional information, please refer to EPA’s Emission Measurement Center website: http://www.epa.gov/ttn/emc/. For

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### copies of the SW- 846 methods, please refer to EPA’s SW -846 Online website: http://www.epa.gov/waste/hazard/testmethods/sw846/index.htm

. If you would like to use a method not listed in Table 1.1, please contact the EPA for approval of an alternative test method. The request for an alternative test method should include the alternative test method or prescriptive alternative procedure, the reason for the request (e.g., lower detection limit, site specific matrix interference, increased precision, etc. ), supporting empirical data (e.g. comparison with specified method, precision determination, etc.), and quality control procedures which ensure results are sufficiently accurate and precise. See the Emission Measurement Center’s Guideline Document 22 ( http://www.epa.gov/ttn/emc/guidlnd/gd22.pdf) for more information on what information should be included in an alternative test method request.

Each test should be comprised of a minimum of three valid runs at each sampling location. All pollutant concentrations should be corrected to 3 percent oxygen and should be reported on the same moisture basis. The target units of measure are specified in Table 1.1. Report the results of each stack test according to the instructions in Section 2.0 of this attachment. 30 days of THC monitoring is also required as specified in Section 1.3. In addition to the emission test data, you must also report the following process information taken during the testing period:

 The type of resin being processed and the resin grade;

 Emissions control device(s) in use during the test;

 Control device operating or monitoring parameters (including, as appropriate to the control device, flue gas flow rate, pressure drop, scrubber liquor pH, scrubber liquor flow rate, sorbent type and sorbent injection rate); and

 Process parameters (such as percent oxygen).

The testing should be conducted while the PVC production process and any other nonPVC production process(es) that send emission streams to the same control device, is/are operating as close as possible to maximum mass loading of all HAP compounds to the control device and under “normal” operation, that is, not during periods of startup, shut down, or malfunction. A thorough description of the process(es), including production rate(s) and a comparison of those production rates to maximum production capacity for PVC process unit s and non-PVC process units during the entire testing cycle should also be provided. If, during the performance testing, it becomes clear that one or more “off specification” or “out of specification” resin batches will be produced, then the testing and process data and any other associated information must still be submitted and labeled as an “off spec” test.

In most instances, we are not specifying numerical detection limits; instead we have specified testing conditions and methods, including test run times and minimum sample volumes when appropriate, which we believe will provide sufficient data quality for decision making. We remind source owners and testers of the Clean Air Act section 114(a)(1) requirement to provide information requested for the development of emissions standards using methods that provide data necessary for the decisions. That includes data of quality sufficient to support those decisions. For the most part, we can identify test methods and procedures that will satisfy those decision making needs (e.g., minimum sampling times). In other cases, we recognize that the source owner's or tester's selection of test procedures or equipment could bear significantly on

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### the quality of the data. See Attachment C of this enclosure for information regarding guidance for calculating and reporting values measured below method detection levels.

We believe that the Clean Air Act is clear that it is incumbent on the source and the tester to apply methods and procedures resulting in data quality necessary for those decisions including providing for the lowest possible detection limits considering practical and reasonable limitations. For example, source owners and testers should not automatically choose to use low or medium quality equipment for testing (e.g., for cost reasons) if high quality equipment is reasonably available. We will review test reports in light of this expectation and will be particularly mindful of whether the testing procedures applied are representative of the highest reasonably expected capabilities (e.g., comparing reported minimum measurement detection levels between tests and testers). If we believe that a source owner or tester has failed to meet the requirement of the Act to provide data sufficient decisions, we can and will request additional measurements requiring the use of improved testing procedures. The enclosed certification statement must be signed by a responsible official (See Enclosure 6).

Table 1.1: Summary of Polyvinyl Chloride and Copolymers’ Control System Outlet Emissions

Measurement Methods and Alternative Methods 1

Pollutant Required Method Possible Al ternative Method Target Reported

Units of Measure Vinyl Chloride U.S. EPA Method 18 with a minimum sample time of 1 hour per run and a nominal detection level of less than 200 ppbv. None pp b vd @ 3% O 2

HCl / Cl 2 U.S. EPA Method 26 or 26A. Collect a minimum sample volume of 2 ds cm per run. None ppmvd @ 3% O 2

THC U.S. EPA Method 25A with a minimum sampling time of 4 hours per run. Calibrate the measuring instrument with a mixture of the organic compounds being emitted or with propane. None p pmvd as propane @ 3 % O 2

CH 4 U.S. EPA Method 320 . Have a minimum sample time of 4 hour s per run. U.S. EPA Method 18. Have a minimum sample time of 4 hour s per run

. ppmvd @ 3 % O 2

Dioxins/Furans 2 U.S. EPA Method 23. Collect a minimum sample volume of 5 dscm per run. Use high resolution GC/MS for the analytical finish. None ng/dscm @ 3% O 2

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Units of Measure Speciated HAP listed in Table 1.3 3 Sample collection by SW

- 846 Method 0031 , sample preparation by SW

- 846 Method 5041A, and sample analysis by SW

- 846 Method 8260B 4

. Combine traps in each run if lower detection limit is needed. Sample at a rate of 1 L/min, unless a slower sampling rate will yield detectable levels. None ppmvd @ 3% O 2

Speciated HAP listed in Table 1.4 3 Sample collection by SW

- 846 Method 0010 , sample preparation by SW

- 846 Method 3542 5 , and sample analysis by SW

- 846 Method 8270D 4 . Collect a minimum sample volume of 3 ds cm per

run . Use low resolution GC / MS with the use of selected ion monitoring (SIM) mode for the analytical finish. None ppmvd @ 3% O 2

Speciated HAP listed in Table 1.5 3 U.S. EPA Method 18 or 320 6

. Minimum s ampl e time of 1 hour per run. All compounds quantified by Method 320 must be validated according to Section 13.0 of Method 320. All compounds quantified by Method 18 meet the recovery study specified in Section 8.4 of Method 18. None ppmvd @ 3% O 2

O 2 / CO 2 U.S. EPA Method 3A. Simultaneous with each pollutant test run. U.S. EPA Method 3B % volume, dry

Moisture U.S. EPA Method 4. Simultaneous with each pollut ant test run. None % volume

Flowrate U.S. EPA Method 2. Simultaneous with each pollutant test run. U.S. EPA Method 2A, 2B, 2C, 2D, 2F, or 2G, as appropriate

. ascfm and dscf m

1 You must sample THC, vinyl chloride, and all speciated HAP concurrently.

2 You must include the results for the individual dioxin/furan congeners as specified in Table 1.2.

3 If any HAP other than those listed in Tables 1.3-1.5 could be emitted from the process, you must test for those HAP using US EPA Method 320, US EPA Method 18

, SW -846 Method 0010, or an approved alternative test method, as applicable

. 4 You must use all three SW-846 methods in combination to obtain a measurement result. The first method is the sampling method to be used at the stack. The second method is a preparatory method that readies for analysis the sample obtained from the first method. The third method is the analysis method.

5 SW -846 Method 3542 replaces Section 8.1 of SW-846 Method 0010.

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– Bag Sampling (Section 8.2.1), Method 18

– Direct Interface (Section 8.2.2), or Method 18

– Absorption Tube (Section 8.2.4 )] must be made for each compound in Table 1.5 to achieve the lowest detection limit and meet method quality parameters.

Table 1.2 Dioxin/Furan Congeners

Dioxin/furan congener

2,3,7,8

- tetrachlorodibenzo

- p

- dioxin.

1,2,3,7,8

- pentachlorodibenzo

- p

- dioxin.

1,2,3,4,7,8

- hexachlorodibenzo

- p

- dioxin.

1,2,3,7,8,9

- hexachlorodibenzo

- p

- dioxin.

1,2,3,6,7,8

- hexachlorodibenzo

- p

- dioxin.

1,2,3,4,6,7,8

- heptachlorodibenzo

- p

- dioxin.

octachlorodibenzo

- p

- dioxin.

2,3,7,8

- tetrachlorodibenzofuran.

2,3,4,7,8

- pentachlorodiben zofuran.

1,2,3,7,8

- pentachlorodibenzofuran.

1,2,3,4,7,8

- hexachlorodibenzofuran.

1,2,3,6,7,8

- hexachlorodibenzofuran.

1,2,3,7,8,9

- hexachlorodibenzofuran.

2,3,4,6,7,8

- hexachlorodibenzofuran.

1,2,3,4,6,7,8

- heptachlorodibenzofuran.

1,2,3,4,7,8,9

- heptachlorodibenzofuran.

Octachlorodibenzofuran.

Table 1.3 Target Analytes Using SW-846 Method 8260B

Pollutant CAS Number Pollutant CAS Number

Benzene 71432 n

- Hexane 110543
Chloroethane 75003 Methylene chloride 75092
Chloroform 67663 Toluene 108883 Chloroprene 126998 1,1,1

- Trichloroethane 71556 1,1

- Dichloroethane 75343 1,1,2

- Trichloroethane 79005 1,2

- Dichloroethane 107062 Vinylidene chloride 75354

Table 1.4 Target Analytes Using SW-846 Method 8270D

Pollutant CAS Number Pollutant CAS Number Acetophenone 98862 Hydroquinone 123319

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- ethylhexyl) phthalate (DEHP) 117817 Naphthalene 91203

1,4

- Dichlorobenzene 106467 Phenol 108952 2,4

- Dinitrophenol 51285 1,2,4

- Trichlorobenzene 120821
Hexachlorobutadiene 87683

Table 1.5 Target Analytes Using US EPA Method 18 and 320

Pollutant CAS Number Pollutant CAS Number Acetaldehyde 75070 Formaldehyde 50000 1,3

- Butadiene 106990 Methanol 67561
Chlorobenzene 108907 1,1,2,2

- Tetrachloroethane 79345
Chloromethane 74873 2,2,4

- Trimethylpentane 540841
Cumene 98828 Vinyl acetate 108054 Ethylbenzene 100414 Vinyl bromide 593602 Ethylene glycol 107211 Xylenes (isomers and mixtures) 1330207



### 1.3 Total Hydrocarbon 30 -Day Monitoring

You must conduct total hydrocarbon (T HC ) monitoring continuously for a 30-day period as specified in Table 1.6. You must also concurrently record the exhaust gas oxygen and moisture levels, the types and grades of PVC resin being produced and the control device temperature. Also indicate periods of abnormal operation for the control device and/or THC monitoring equipment. All the emissions testing required in Table 1.1 must be conducted during this 30-day monitoring period.

Table 1.6 30-Day THC Monitoring

Pollutant Recommended Method Alternati ve Method Target Reported Units of Measure
THC U.S. EPA Method 25A

continuously for 30 days. Calibrate the measuring instrument with propane. The low level and high level calibration gases (see sections 7.1.3 and 7.1.5 of Method 25A) must bracket the mea sured concentrations or a maximum high level calibration gas (see section 7.1.5 of Method 25A) of 10 ppm propane must be used. None ppmvd as propane @ 3% O 2

CH 4 U.S. EPA Method 320 U.S. EPA Method 18 or instrument that uses chromatographic column to split methane from all other organic compounds. ppmvd @ 3% O 2

O 2 U.S. EPA Method 3A

continuously for 30 days. U.S. EPA Method 3B % volume, dry

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Moisture U.S. EPA Method 4 once per

day fo r 30 days

. W here the exhaust stream is saturated (e.g. the outlet of a wet scrubber), you may measure the temperature by thermocouple and report the moisture at saturation levels. W here a stack is not saturated

, moisture may be determined by wet/dry bulb psychrometry (ASTM E

- 337) twice daily (at least one hour apart)

, by Met hod 320

, or by ASTM D6348

- 12 (FTIR) % volume



### 2 .0 How to Report Data

The method for reporting the results of testing and monitoring depends up on the methods used to complete the testing and monitoring requirements. This section discusses the requirements for reporting the collected data.

2.1 Reporting stack test data

For data collected using EPA Methods 23, 25/25A, and 26/26A, you must report the results of the performance test using the EPA’s Elect ronic Reporting Tool (ERT). You do not need to use the ERT to report the results of the 30-d ay THC monitoring; you only need to use the ERT to report the results of the Table 1.1 stack test. The ERT website (see http://www.epa.gov/ttn/chief/ert/index.htm l) contains the latest version of the ERT, as well as frequently asked questions and a user’s guide. The ERT is a Microsoft Access program that must be downloaded onto your computer prior to data entry. The file generated from the ERT must be submitted according to one of the methods specified in Section 3.0 of this Attachment.

For data collected using all other test methods, you must report the results of the performance test(s) using Form P in the information collection request response forms Microsoft Excel workbook. You must also submit an electronic copy of the emission test report that includ es all of the information specified in Section 2.2 of this Attachment (PDF format preferred).

If you claim that some of the results of the performance test being submitted are confidential business information (CBI), you must submit the complete file including information claimed to be CBI. The submitted materials must be clearly marked as CBI submitted according to Section 3.0 of this Attachment. You must submit a separate copy of the file with all CBI data removed. Submit the non-CBI version of the file according to one of the options in Section 3.0 of this Attachment.

2.2 Stack test data to be included in the report

At a minimum, all performance test reports must include the following information:

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###  General identification information for the facility including a mailing address, the actual address, the owner or operator or responsible official (where they are applicable) or an appropriate representative and an email address for this person, and the appropriate Federal Registry System (FRS) number for the facility;

 A brief process description, including a flow diagram clearly showing all process ventpiping at the inlet to the first control device including manifolds and tie-in points for nonPVC process unit process vents (with those non-PVC process units identified), any piping that allows a process vent to bypass the control device(s), and the sampling site;

 A complete unit description for PVC and non-PVC process units, including a description of emission streams and control devices, the appropriate source classification code (SCC), the latitude and longitude of the emission point being tested (to five decimal points), and the permitted maximum process rate (where applicable);

 Sampling site description; description of sampling and analysis procedures and any modifications to standard procedures; quality assurance procedures;

 Any process data and control device monitoring data required in this attachment;

 Raw data sheets for field sampling;

 Raw data sheets for field and laboratory analyses;

 Chain-of-custody documentation;

 Explanation of laboratory data qualifiers;

 Example calculations of all applicable stack gas parameters, emission rates, percent reduction rates, and analytical results, as applicable;

 Identification information for the company conducting the performance test including a contact person and his/her email address; and

 Any other information required by the test method, a relevant standard, or the Administrator.

Make clear, using the “ Notes ” section of the ERT or Form P, the correlation between emissions measurements and process data (e.g., identify Method 29, run 1 for the associated process data on the process data details tab of the ERT).

2. 3 Flagging data and handling data that is below the detection limit

See Attachment C of this enclosure for information on how to flag data and on how to calculate and report values measured below the method detection limit.

3.0 How to Submit Data

You may submit your data in one of the three ways listed below. However, in order to avoid duplicate data and keep all data for a particular facility together, we request that you submit all non

- CBI data requested from your facility in the same way. To submit your data:

 

### E-mail an electronic copy of all requested files to CCG -PVC@epa.gov

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### Mail a CD or DVD containing an electronic copy of all requested files to the EPA address shown in your section 114 letter. If no electronic copy is available, mail a hard copy of all requested files to the EPA address shown in your section 114 letter.

 

### If you are submitting Confidential Business Information (CBI), you must mail a separate CD or DVD containing only the CBI portion of your data to the EPA address shown in your section 114 letter.

4 .0 Contact Information for Questions

For questions on how to report data using the ERT contact:

Ron Myers (919) 541 -5407 myers.ron@epa.gov

For questions on the test methods contact:

Jason DeWees (919) 541 -9724 dewees.jason@epa.gov

Stef Johnson (919) 541 -4790 johnson.steffan@epa.gov

For all other questions contact:

Jodi Howard (919) 541 -4607 howard.jodi@epa.gov

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## Guidance for Calculating and Reporting Values Measured Below Method Detection Levels

1.0 Identification of Detection Levels

Identify the status of measured values relative to detection levels on the spreadsheet or in the ERT using the following descriptions:

 BDL (below detection level)

– all analytical values used to calculate and report an instack emissions value are less than the laboratory’s reported detection level(s);

 DLL (detection level limited)

– at least one but not all values used to calculate and report an in- stack emissions value are less than the laboratory’s reported detection level(s); or

 ADL (above detection level)

– all analytical values used to calculate and report an instack emissions value are greater than the laboratory’s reported detection level(s).

2.0 Reporting and Calculating Method Detection Limits

For reporting and calculating individual test run data:

 You must use the method specified approach for calculation and determination of the method detection limit (MDL). If the method does not specify the approach and calculation of the MDL, determine the MDL as follows:

o For air sampling and analysis methods, you must determine the MDL in accordance with the procedures specified in Section 15 of Method 301 (located in Appendix A of 40 CFR part 63).

o For water sampling and analysis, you must determine the MDL in accordance with the procedures specified in Appendix B of 40 CFR part 136.

 For analytical data reported from the laboratory as above the MDL, include the ADL flag in the Form P columns labeled “ Run #1 Detection”, “ Run #2 Detection”, and/or “ Run #3 Detection” as appropriate or in the Comments line in the ERT.

 For analytical data reported from the laboratory as “nondetect” or “below detection level;”

o Include a brief description of the procedures used to determine the analytical detection and in-stack detection levels:

 In the Notes line of Excel spreadsheet template; or

 In the Comments line of Lab Data tab in the Run Data Details in the ERT.

o Describe these procedures completely in the full test report including the measurements made, the standards used, and the statistical procedures applied.

o Calculate the in-stack emissions rate for any analytical result reported as below detection level using the relevant MDL, sampling volumes and other relevant run

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### specific parameters (such as oxygen or flowrate). The reported value must assume that the analyte is present at the full MDL value.

o Report the calculated emissions concentration or rate result:

 As a detection level numerical value (i.e., no brackets or < symbol) in the Excel spreadsheet template (Form P; columns “ Run 1”, “ Run 2”, and/or

“ Run 3” as appropriate) and select the appropriate flag in the Form P columns labeled “ Run #1 Detection”, “ Run #2 Detection”, and/or “ Run #3 Detection” as appropriate ; or

 As a numerical value in the ERT with the appropriate flag in the Comments line.

o Report as numerical values (i.e., no brackets or < symbol) any analytical datameasured above the MDL, including any data between the MDL and a laboratoryspecific reporting or quantification level (i.e., flag as ADL).

o Apply these reporting and calculation procedures to measurements made with Method 23 :

 Report data in the ERT for each of the D/F congeners measured with Method 23 below the detection level as [< detection level];

 Do not report emissions as zero, as described in the method.

 For pollutant measurements composed of multiple components or fractions (e.g., Hg and other metals sampling trains) when the result for the value for any component is measured below the MDL:

o Calculate in-stack emissions rate or concentrations as outlined above for each component or fraction;

o Sum the measured values and/or calculated values (using the MDL as outlined above) for all of the components or fractions; and

o Report the sum of all components or fractions:

 As a detection level numerical value (i.e., no brackets or < symbol) in the Excel spreadsheet template (Form P; columns “ Run 1”, “ Run 2”, and/or

“ Run 3” as appropriate) and select the appropriate flag in the Form P columns labeled “ Run #1 Detection”, “ Run #2 Detection”, and/or “ Run #3 Detection” as appropriate ; or

 As a numerical value in the ERT with the appropriate flag in the Comments line.

 If all components or fractions are BDL, the appropriate flag is BDL. If any component or fraction is ADL, the appropriate flag is DLL.

o In addition to reporting the sum of the components or fractions, report the individual component or fraction values for each run if the Excel spreadsheet template or ERT format allows.

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### o If the Excel spreadsheet template or ERT format does not allow reporting of the individual components or factions (i.e., the format allows reporting only a single sum value):

 For the Excel spreadsheet template, next to the sum reported as above

rep ort in the Notes line the appropriate flag along with the values for the measured or MDL value for each component or fraction as used in the calculations (e.g., 0.036, [<0.069], 1.239, [<0.945] for a four fraction sample)

 For the ERT, next to the sum reported as above, report on the Comments line the appropriate flag and the measured or MDL value for each component or fraction as used in the calculations (e.g., 0.036, [<0.069], 1.239, [<0.945] for a four fraction sample)

 For measurements conducted using instrumental test methods (e.g., Methods 3A, 6C, 7E, 10, 25A):

o Record gaseous concentration values as measured including negative values and flag as ADL; do not report as BDL

o Calculate and report in-stack emissions rates using these measured values

o Include relevant information relative to calibration gas values or other technical qualifiers for measured values in Comments line in the ERT or Notes line of the Excel spreadsheet.

 For reporting and calculating average emissions rate or concentration for a test when some results are reported as BDL:

o Sum all of the test run values including those indicated as BDL or DLL as numerical values

o Calculate the average emissions rate or concentration (e.g., divide the sum by 3 for a three-run test)

o Report the average emissions rate or concentration average:

 As a detection level numerical value (i.e., no brackets or < symbol) in the Excel spreadsheet template (Form P; columns “ Run 1”, “ Run 2”, and/or

“ Run 3” as appropriate) and select the appropriate flag in the Form P columns labeled “ Run #1 Detection”, “ Run #2 Detection”, and/or “ Run #3 Detection” as appropriate;

 As a numerical value in the ERT and include the appropriate flag in the relevant Comments line

 If all test run values are BDL, the appropriate flag is BDL. If any test run value is ADL or DLL, the appropriate flag is DLL.